CN108241033A - The method of 6 quality index content of material and application in a kind of quick detection Radix Ophiopogonis alcohol extract - Google Patents
The method of 6 quality index content of material and application in a kind of quick detection Radix Ophiopogonis alcohol extract Download PDFInfo
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- CN108241033A CN108241033A CN201810035604.8A CN201810035604A CN108241033A CN 108241033 A CN108241033 A CN 108241033A CN 201810035604 A CN201810035604 A CN 201810035604A CN 108241033 A CN108241033 A CN 108241033A
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- quality index
- radix ophiopogonis
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- alcohol extract
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- 238000000034 method Methods 0.000 title claims abstract description 88
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000000284 extract Substances 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000001514 detection method Methods 0.000 title claims abstract description 14
- UFMAZRUMVFVHLY-CYBMUJFWSA-N (3r)-5,7-dihydroxy-3-[(4-methoxyphenyl)methyl]-6,8-dimethyl-2,3-dihydrochromen-4-one Chemical compound C1=CC(OC)=CC=C1C[C@H]1C(=O)C2=C(O)C(C)=C(O)C(C)=C2OC1 UFMAZRUMVFVHLY-CYBMUJFWSA-N 0.000 claims abstract description 40
- BXTNNJIQILYHJB-GFCCVEGCSA-N Methylophiopogonanone A Chemical compound C1=C2OCOC2=CC(C[C@@H]2COC3=C(C)C(O)=C(C(=C3C2=O)O)C)=C1 BXTNNJIQILYHJB-GFCCVEGCSA-N 0.000 claims abstract description 36
- 229930182490 saponin Natural products 0.000 claims abstract description 29
- 150000007949 saponins Chemical class 0.000 claims abstract description 29
- 235000017709 saponins Nutrition 0.000 claims abstract description 29
- 238000001228 spectrum Methods 0.000 claims abstract description 26
- 240000002948 Ophiopogon intermedius Species 0.000 claims abstract description 25
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 23
- 229930091371 Fructose Natural products 0.000 claims abstract description 22
- 239000005715 Fructose Substances 0.000 claims abstract description 22
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims abstract description 22
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 21
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 20
- 229930006000 Sucrose Natural products 0.000 claims abstract description 20
- 239000008103 glucose Substances 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 18
- 239000005720 sucrose Substances 0.000 claims abstract description 11
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 10
- 238000012795 verification Methods 0.000 claims description 26
- 229960004793 sucrose Drugs 0.000 claims description 19
- 239000008862 fructus schizandrae, radix ginseng, radix ophiopogonis drug combination Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 238000002347 injection Methods 0.000 claims description 15
- 239000007924 injection Substances 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 12
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- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 7
- 238000004611 spectroscopical analysis Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000000105 evaporative light scattering detection Methods 0.000 claims description 5
- 238000000491 multivariate analysis Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 241000209140 Triticum Species 0.000 claims description 3
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- 239000008121 dextrose Substances 0.000 claims description 3
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000013558 reference substance Substances 0.000 description 11
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- 238000005457 optimization Methods 0.000 description 7
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- 150000001720 carbohydrates Chemical class 0.000 description 6
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- 235000014633 carbohydrates Nutrition 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 240000000111 Saccharum officinarum Species 0.000 description 3
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- 238000002835 absorbance Methods 0.000 description 3
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- 150000001875 compounds Chemical class 0.000 description 3
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- 241000208340 Araliaceae Species 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 235000002789 Panax ginseng Nutrition 0.000 description 2
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QMQIQBOGXYYATH-IDABPMKMSA-N Ruscogenin Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)[C@H](O)C[C@H](O)CC4=CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 QMQIQBOGXYYATH-IDABPMKMSA-N 0.000 description 2
- BSUPFYRQXCQGLJ-UHFFFAOYSA-N Ruscogenin Natural products CC1CCC2(OC1)OC3C(O)C4C5CC=C6CC(O)CC(O)C6(C)C5CCC4(C)C3C2C BSUPFYRQXCQGLJ-UHFFFAOYSA-N 0.000 description 2
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- QMQIQBOGXYYATH-UHFFFAOYSA-N epiruscogenin Natural products CC1C(C2(CCC3C4(C)C(O)CC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 QMQIQBOGXYYATH-UHFFFAOYSA-N 0.000 description 2
- 238000010812 external standard method Methods 0.000 description 2
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- 229930003944 flavone Natural products 0.000 description 2
- 150000002213 flavones Chemical class 0.000 description 2
- 235000011949 flavones Nutrition 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 235000008434 ginseng Nutrition 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
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- 229940109990 ruscogenin Drugs 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- DQYACEDUQHWXQZ-UHFFFAOYSA-N (25R)-spirost-5-en-3beta-ol 3-O-<O-alpha-L-rhamnopyranosyl-(1-2)-O-<alpha-L-arabinopyranosyl-(1-3)>-beta-D-glucopyranoside> Natural products O1C2(OCC(C)CC2)C(C)C(C2(CCC3C4(C)CC5)C)C1CC2C3CC=C4CC5OC(C1OC2C(C(O)C(O)C(C)O2)O)OC(CO)C(O)C1OC1OCC(O)C(O)C1O DQYACEDUQHWXQZ-UHFFFAOYSA-N 0.000 description 1
- FHKHGNFKBPFJCB-UHFFFAOYSA-N (25S)-ruscogenin 1-O-<alpha-L-rhamnopyranosyl(1->2)><beta-D-xylopyranosyl(1->3)>-beta-D-fucopyranoside Natural products O1C2(OCC(C)CC2)C(C)C(C2(CCC3C45C)C)C1CC2C3CC=C4CC(O)CC5OC(C1OC2C(C(O)C(O)C(C)O2)O)OC(C)C(O)C1OC1OCC(O)C(O)C1O FHKHGNFKBPFJCB-UHFFFAOYSA-N 0.000 description 1
- MQTJXIHSKXORQL-RFMZWHELSA-N 911819-08-4 Chemical compound O([C@H]1[C@@H](O)[C@@H](C)O[C@@H]([C@@H]1O[C@H]1[C@@H]([C@H](O)[C@@H](O)[C@H](C)O1)O)O[C@@H]1C[C@@H](CC2=CC[C@H]3[C@@H]4C[C@H]5[C@@H]([C@]4(CC[C@@H]3[C@]21C)C)[C@@H]([C@]1(OC[C@H](C)CC1)O5)C)OC(C)=O)[C@@H]1OC[C@@H](O)[C@H](O)[C@H]1O MQTJXIHSKXORQL-RFMZWHELSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 206010019280 Heart failures Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- FHKHGNFKBPFJCB-LYLKFOBISA-N Ophiopogonin D Chemical compound O([C@H]1[C@@H](O)[C@@H](C)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@H](O)[C@@H](O)[C@H](C)O1)O)O[C@@H]1C[C@H](O)CC2=CC[C@H]3[C@@H]4C[C@H]5[C@@H]([C@]4(CC[C@@H]3[C@]21C)C)[C@@H]([C@]1(OC[C@H](C)CC1)O5)C)[C@@H]1OC[C@@H](O)[C@H](O)[C@H]1O FHKHGNFKBPFJCB-LYLKFOBISA-N 0.000 description 1
- NJYZGIOABZGGBB-UHFFFAOYSA-N Ophiopogonin D' Natural products CC1CCC2(OC1)OC3CC4C5CC=C6CC(CCC6(C)C5CCC4(C)C3C2C)OC7OC(CO)C(O)C(OC8OCC(O)C(O)C8OC9OC(C)C(O)C(O)C9O)C7O NJYZGIOABZGGBB-UHFFFAOYSA-N 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical group O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- LKDRXBCSQODPBY-ZXXMMSQZSA-N alpha-D-fructopyranose Chemical compound OC[C@]1(O)OC[C@@H](O)[C@@H](O)[C@@H]1O LKDRXBCSQODPBY-ZXXMMSQZSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000000118 anti-neoplastic effect Effects 0.000 description 1
- 206010003119 arrhythmia Diseases 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
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- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 230000002218 hypoglycaemic effect Effects 0.000 description 1
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- 150000002772 monosaccharides Chemical class 0.000 description 1
- 208000031225 myocardial ischemia Diseases 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 229930190017 ophiopogonin Natural products 0.000 description 1
- IDGCVTONMQMXPU-JHZREZMDSA-N ophiopogonin D Natural products C[C@@H]1CC[C@@]2(OC1)O[C@H]3C[C@H]4[C@@H]5CC=C6C[C@@H](O)C[C@@H](O[C@@H]7O[C@H](CO)[C@@H](O)[C@H](O[C@@H]8OC[C@@H](O)[C@H](O)[C@H]8O)[C@H]7O[C@@H]9O[C@@H](C)[C@H](O)[C@@H](O)[C@H]9O)[C@]6(C)[C@H]5CC[C@]4(C)[C@H]3[C@@H]2C IDGCVTONMQMXPU-JHZREZMDSA-N 0.000 description 1
- KLOUOGJUAFMUDK-DGDLHAQSSA-N ophiopojaponin C Natural products C[C@@H]1[C@@]2(CC[C@@H](C)CO2)O[C@H]2C[C@@]3(O)[C@@H]4CC=C5C[C@H](CC[C@]5(C)[C@H]4CC[C@]3(C)[C@@]12O)O[C@@H]1O[C@H](CO)[C@@H](O[C@@H]2OC[C@@H](O)[C@H](O)[C@H]2O)[C@H](O)[C@H]1O[C@@H]1O[C@@H](C)[C@H](O)[C@@H](O)[C@H]1O KLOUOGJUAFMUDK-DGDLHAQSSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000003182 parenteral nutrition solution Substances 0.000 description 1
- 238000010238 partial least squares regression Methods 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 239000012898 sample dilution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- DKVBOUDTNWVDEP-NJCHZNEYSA-N teicoplanin aglycone Chemical compound N([C@H](C(N[C@@H](C1=CC(O)=CC(O)=C1C=1C(O)=CC=C2C=1)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)OC=1C=C3C=C(C=1O)OC1=CC=C(C=C1Cl)C[C@H](C(=O)N1)NC([C@H](N)C=4C=C(O5)C(O)=CC=4)=O)C(=O)[C@@H]2NC(=O)[C@@H]3NC(=O)[C@@H]1C1=CC5=CC(O)=C1 DKVBOUDTNWVDEP-NJCHZNEYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of methods of 6 quality index content of material in quick detection Radix Ophiopogonis alcohol extract, belong to Chinese Traditional Medicine quality-monitoring field.The method includes：(1) collection of calibration set sample；(2) content of fructose in calibration set sample, glucose, sucrose, dwarf lilyturf tuber total saponins, Methylophiopogonanone A B and methylophiopogonanone B is measured using conventional method；(3) measure of calibration set sample ultra-violet absorption spectrum；(4) calibration model is established；(5) calibration model is verified；(6) 6 quality index content of material of Radix Ophiopogonis alcohol extract to be measured are calculated.The present invention is easy to operate, compared with traditional analysis method, shortens 50 times of total minute or more.There are preferable correlations between ultraviolet characteristic spectrum and the content of 6 different quality index substances, ensure the completion quality of abstraction process, and then ensure end product quality by monitoring quality index in real time.
Description
Technical field
The present invention relates to Chinese Traditional Medicine quality-monitoring fields, and in particular in a kind of quick detection Radix Ophiopogonis alcohol extract
It the method for 6 quality index content of material and its is measured among Radix Ophiopogonis alcohol extracting unit simultaneously in Shenmai injection production process
Application in body in 6 quality index.
Background technology
Shenmai injection is the pure Chinese medicine quick-effective preparation developed on the basis of traditional Chinese medical science ancient prescription " Shengmai San " through remodeling, by red ginseng
It is made with two taste medicinal material of Radix Ophiopogonis through alcohol extracting-water precipitating technique.Clinically, Shenmai injection is mainly used for heart failure, cardiac arrhythmia
Etc. angiocardiopathies treatment, be in addition also commonly used for the adjuvant drug of antineoplastic.With the extensive use of Shenmai injection, people
Increasingly pay close attention to its production process quality control level.
Saponin component and homoisoflavone constituents in Radix Ophiopogonis are the important substance bases of its prevention and cure of cardiovascular disease, are had
It resists myocardial ischemia, is hypoglycemic, anti-aging, inhibiting the physiological activity such as tumour, immunological regulation.But simultaneously containing a large amount of single in Radix Ophiopogonis
Sugar, disaccharide and oligosaccharide, the presence of these carbohydrates bring the stability of Shenmai injection, safety and quality control very greatly
Risk, directly affect the parameters such as parenteral solution osmotic pressure, amount of solid.To sum up, the quality control level of this few class substance is improved
It is significant to the Quality Control level for improving Shenmai injection production process entirety.
In the production process of SHENMAI ZHUSHEJI, Radix Ophiopogonis alcohol reflux extracting process unit can extract the soap in Radix Ophiopogonis
The ingredients such as glycoside, flavonoids and monosaccharide, disaccharides, alcohol extract complicated component, quality control are worth being paid close attention to and being studied.It is real
In the production process of border, the assay method of ophiopogonin class, flavonoids and carbohydrate content is different in intermediate.Application publication number
Patent document for CN105004830A discloses high performance liquid chromatography side that is a kind of while measuring 5 kinds of saponin constituents in Radix Ophiopogonis
Method, 5 kinds of saponin constituents for Ophiopojaponin-C, deacetylate Ophiopojaponin-A, 3-O- α-L- rhamnoses-
(1 → 2)-β-glucose Radix Ophiopogonis aglycon, ophiopogonin D and ophiopogonin D '.Application publication number is the patent of CN 105301130A
Disclose a kind of efficient liquid-phase chromatography method for detecting flavones content in Radix Ophiopogonis；Application publication number is the special of CN 102133333A
Profit discloses a kind of quality control method for shenmai injection mass spectrum finger prints, liquid chromatogram is used as separation means, with mass spectrum
Detector obtains red ginseng and two kinds of finger-prints of Radix Ophiopogonis compound information in characterization Shenmai injection simultaneously for detection means, adopts
Similarity is calculated with correlation coefficient process, is judged as the product of stable quality with the sample of similarity >=0.9.
Above method analysis precision is higher, but analysis personnel is needed to take a significant amount of time and are analyzed it, method analysis
It is complicated for operation, appliance time is long, pretreatment is troublesome, high to instrument and analysis personnel requirement, be not suitable for the real-time analysis of process
With monitoring.
Invention content
The purpose of the present invention is to provide one kind can simultaneously, quickly detect 6 quality index objects in Radix Ophiopogonis alcohol extracting thing
Matter fructose, glucose, sucrose, dwarf lilyturf tuber total saponins, Methylophiopogonanone A B and methylophiopogonanone B contain
The method of amount, and apply it to the reality of 6 quality index in Shenmai injection production process Radix Ophiopogonis alcohol reflux extraction unit
When monitoring and Radix Ophiopogonis alcohol extracting process on-line monitoring in.
To achieve the above object, the present invention adopts the following technical scheme that：6 matter in a kind of quick detection Radix Ophiopogonis alcohol extract
The method of figureofmerit content of material, 6 quality index substances are fructose, glucose, sucrose, dwarf lilyturf tuber total saponins, methyl wheat
Winter Homoisoflavonoids A and methylophiopogonanone B, which is characterized in that this method includes the following steps：
(1) calibration set sample is collected：The Radix Ophiopogonis of different batches is selected, is received in the different phase of Radix Ophiopogonis alcohol reflux extraction process
The Radix Ophiopogonis alcohol extract of collection is as calibration set sample；
(2) 6 quality index substance reference points of calibration set sample measure：A, using high performance liquid chromatography and evaporative light-scattering
Detector combination method measures the content of fructose, dextrose and saccharose；B, containing using perchloric acid determination of color dwarf lilyturf tuber total saponins
Amount；C, Methylophiopogonanone A B and methyl Radix Ophiopogonis dihydro Gao Yi are measured using high performance liquid chromatography-ultraviolet light detection method
The content of flavones B；
(3) measure of calibration set sample ultra-violet absorption spectrum：Using the quartz colorimetric utensil of light path 10mm, by calibration set sample
Dilution, which is placed in ultraviolet-visual spectrometer, carries out full wavelength scanner, and wavelength scanning range is 190~800nm, and scanning accuracy is
1nm, using water as blank solution, each sample makees 3 parallel sweeps, takes ultravioletvisible absorption of the average spectroscopic data as sample
Spectroscopic data obtains calibration set sample ultraviolet-visible absorption spectroscopy data；
(4) calibration model is established：Using multivariate data analysis method, 6 quality index substances in calibration set sample are established
The mathematical model of relationship between content and corresponding ultraviolet-visible absorption spectroscopy, related coefficient >=0.9 of the calibration model；
(5) calibration model is verified：The calibration model that step (4) is established using leaving-one method is intersected and carries out internal verification,
The method of verification is to take Radix Ophiopogonis alcohol extract to be measured, measures its ultraviolet-visible absorption spectroscopy, is inputted each quality index substance
Calibration model in, the content of corrresponding quality index substance in calculating, with the Radix Ophiopogonis alcohol extract according to step (2) method measure
Each quality index content of material compare, it is desirable that measurement error be less than or equal to 25%；
(6) 6 quality index content of material of Radix Ophiopogonis alcohol extract to be measured are calculated：6 quality index substances to be measured is taken to contain
The winter wheat extracting solution sample of amount is inhaled according to the UV, visible light of the ultraviolet spectra acquisition method collecting sample identical with calibration set sample
Spectral information is received, which is inputted in the calibration model of each quality index substance, calculates corrresponding quality in sample to be tested
The content of index substance.
Present invention multivariate data analysis method described in step (4) is principal component regression method or Partial Least Squares.
The present invention is used as calibration set sample by collecting representative Radix Ophiopogonis alcohol extract, with certain acquisition mode
Scanning obtains the ultraviolet-visible absorption spectroscopy figure of calibration set sample.Fructose, Portugal in calibration set sample are measured with traditional quantitative methods
Grape sugar, sucrose, dwarf lilyturf tuber total saponins, Methylophiopogonanone A B and methylophiopogonanone B content as ginseng
According to value, using the PCR methods and PLS methods in multivariate data analysis technology, the ultraviolet spectra and its matter of Radix Ophiopogonis alcohol extract are established
The multivariate calibration model of relationship between figureofmerit by Radix Ophiopogonis extract to be measured, measures its ultraviolet spectra after the same method,
Each quality indicator value can quickly be calculated using the calibration model built.
Compared with prior art, the advantageous effect that the present invention has：
(1) ultraviolet light spectrum quick test Shenmai injection production process Radix Ophiopogonis alcohol extracting unit intermediate provided by the invention
The method of 6 quality index, easy to operate, quick, pretreatment is simple.Compared with traditional analysis method, shorten minute
50 times or more, and a large amount of organic solvent is not needed to, meet the theory of green manufacturing.
(2) there are preferable correlation between ultraviolet-visible absorption spectroscopy and the content of 6 different quality index substances,
The problem of contents of each constituents in Radix Ophiopogonis alcohol extract is difficult to quickly be measured can be efficiently solved, by monitoring quality in real time
Index carries out real-time process monitoring, ensures the completion quality of abstraction process, and then ensure end product quality, can be in Chinese medicine system
It is promoted and applied in agent production.
Description of the drawings
Fig. 1 is the flow diagram of the present invention.
Fig. 2 is the ultraviolet spectrogram of Radix Ophiopogonis alcohol extract calibration set sample.
Fig. 3 is Radix Ophiopogonis alcohol extract calibration set sample through SG is smooth and the pretreated spectrogram of first derivation.
Fig. 4 is the dwarf lilyturf tuber total saponins content PCR quantitative model reference points of Radix Ophiopogonis alcohol extract verification collection and calibration set sample
Correlativity figure between predicted value.
Fig. 5 is that Radix Ophiopogonis alcohol extract verification collection and the Methylophiopogonanone A B content PCR of calibration set sample are quantified
Correlativity figure between the reference point and predicted value of model.
Fig. 6 is that Radix Ophiopogonis alcohol extract verification collection and the methylophiopogonanone B content PCR of calibration set sample are quantified
Correlativity figure between the reference point and predicted value of model.
Fig. 7 be Radix Ophiopogonis alcohol extract verification collection with the reference point of the fructose content PCR quantitative models of calibration set sample with it is pre-
Correlativity figure between measured value.
Fig. 8 be Radix Ophiopogonis alcohol extract verification collection with the reference point of the glucose content PCR quantitative models of calibration set sample with
Correlativity figure between predicted value.
Fig. 9 be Radix Ophiopogonis alcohol extract verification collection with the reference point of the cane sugar content PCR quantitative models of calibration set sample with it is pre-
Correlativity figure between measured value.
Figure 10 is Radix Ophiopogonis alcohol extract calibration set sample through SG is smooth and the pretreated spectrogram of second order derivation.
Figure 11 be Radix Ophiopogonis alcohol extract dwarf lilyturf tuber total saponins content PLS quantitative model calibration set sample reference point and predicted value it
Between correlativity figure.
Figure 12 is the reference of Radix Ophiopogonis alcohol extract Methylophiopogonanone A B content PLS quantitative model calibration set sample
Correlativity figure between value and predicted value.
Figure 13 is the reference of Radix Ophiopogonis alcohol extract methylophiopogonanone B content PLS quantitative model calibration set sample
Correlativity figure between value and predicted value.
Figure 14 is the phase between the reference point of Radix Ophiopogonis alcohol extract fructose content PLS quantitative model calibration set sample and predicted value
Close relational graph.
Figure 15 is between the reference point of Radix Ophiopogonis alcohol extract glucose content PLS quantitative model calibration set sample and predicted value
Correlativity figure.
Figure 16 is the phase between the reference point of Radix Ophiopogonis alcohol extract cane sugar content PLS quantitative model calibration set sample and predicted value
Close relational graph.
Figure 17 be Radix Ophiopogonis alcohol extract dwarf lilyturf tuber total saponins content PLS quantitative model verification collection sample reference point and predicted value it
Between correlativity figure.
Figure 18 is the reference of Radix Ophiopogonis alcohol extract Methylophiopogonanone A B content PLS quantitative model verification collection sample
Correlativity figure between value and predicted value.
Figure 19 is the reference of Radix Ophiopogonis alcohol extract methylophiopogonanone B content PLS quantitative model verification collection sample
Correlativity figure between value and predicted value.
Figure 20 is the phase between the reference point of Radix Ophiopogonis alcohol extract fructose content PLS quantitative model verification collection sample and predicted value
Close relational graph.
Figure 21 is between the reference point of Radix Ophiopogonis alcohol extract glucose content PLS quantitative model verification collection sample and predicted value
Correlativity figure.
Figure 22 is the phase between the reference point of Radix Ophiopogonis alcohol extract cane sugar content PLS quantitative model verification collection sample and predicted value
Close relational graph.
In Fig. 4 to Fig. 9, the data point of sample 1,9,16 is verification collection sample in figure, remaining is calibration set sample.
In Figure 11 to Figure 16, sample md2, md3 in figure, md4, md5, md6, md7, md8, md10, md11, md12,
The data point of md13, md14, md15, md17 are calibration set sample.
In Figure 17 to Figure 22, the data point of sample md1, md9, md16 are verification collection sample in figure.
Specific embodiment
It is further described with reference to the accompanying drawings and examples, but the present invention is not limited thereto.
Embodiment 1：
Method flow is referring to Fig. 1.
1. the collection of calibration set sample：
30g Radix Ophiopogonis medicine materical crude slice accurately is weighed, is placed in glass jacket extractor, adds in alcoholic solution as Extraction solvent, heating
Refluxing extraction collects filtrate afterwards for a period of time, repeats above step, and a medicine materical crude slice is total to refluxing extraction 2 times, different batches Radix Ophiopogonis second
The ethanol consumption of alcohol reflux extraction process, determining alcohol and single-trial extraction time are different.It is extracted from 10 batch Radix Ophiopogonis alcohol refluxs
Extracting solution is drawn in not timing in technical process, obtains 14 parts of calibration set samples altogether；
2. the measure of calibration set sample fructose, glucose and cane sugar content reference point
It is measured in calibration set sample using high performance liquid chromatography and evaporative light scattering detector combination method (HPLC-ELSD methods)
Fructose, glucose, three kinds of carbohydrates of sucrose content；
(1) analysis condition：Chromatographic column is Grace Prevail Carbonhydrate ES (4.6mm × 250mm, 5 μm),
Mobile phase is acetonitrile-water (70:30), flow velocity 1mL/min, 30 DEG C of column temperature, 10 μ L of sample size；ELSD detector conditions are：Nitrogen
Throughput 2.0L/min；100 DEG C of drift tube temperature；Gain 2.0；Impinger：It closes；
(2) preparation of reference substance solution：Precision weighs fructose, glucose, control sucrose product in volumetric flask, with 50% color
The solution of 10.66mg/mL containing fructose, glucose 4.24mg/mL, sucrose 4.04mg/mL is made to scale in spectrum level methanol dilution,
As mixed reference substance solution 1；Reference substance solution No. 1 5.0mL, 2.5mL, 2.0mL, 1.0mL are accurately pipetted respectively in 10mL
In volumetric flask, scale is diluted to as mixed reference substance solution No. 2, No. 3, No. 4, No. 5 using 50% hplc grade methanol；
(3) standard curve determination：1~No. 5 standard solution is injected into high performance liquid chromatograph respectively, by step (1)
Condition is measured, and carries out linear regression with the logarithm of chromatographic peak area A and the logarithm of reference substance sample introduction quality m, respectively
The standard curve of fructose, glucose and sucrose is drawn, the standard curve of carbohydrate is as shown in table 1；
Regression analysis standard curve, related coefficient and the range of linearity of 1 carbohydrate of table
(4) fructose, dextrose and saccharose assay：Calibration set sample is taken, after 0.45 μm of filtering with microporous membrane, is taken continuous
Filtrate injects liquid chromatograph, is measured by step (1) conditional, three kinds of contents of saccharide is calculated by external standard method, as reference
Value.
3. the measure of calibration set sample total saponin content reference point
It, can with Lu Si containing dwarf lilyturf tuber total saponins using the content of dwarf lilyturf tuber total saponins in perchloric acid determination of color calibration set sample
Sapogenin meter；
(1) preparation of reference substance solution：Take ruscogenin reference substance appropriate, it is accurately weighed, add methanol that every 1mL is made
Solution containing 120 μ g to get；
(2) preparation of standard curve：Precision measure reference substance solution 0.2mL, 0.5mL, 1.0mL, 2.0mL, 3.0mL,
4.0mL is put in tool plug test tube respectively, and solvent is volatilized in water-bath, and precision adds in perchloric acid 10mL, shakes up, kept the temperature in hot water
It is taken out after 15 minutes, ice water cooling, using corresponding reagent as blank, according to UV-VIS spectrophotometry, (Chinese Pharmacopoeia 2015 editions is attached
Record V A), absorbance is measured at 397nm wavelength, standard curve is drawn to concentration c with absorbance A, calibration curve formula is as follows：
A=12.994c-0.0193, R2=0.9957, range of linearity 0.0012-0.0480mg/mL；
(3) measuring method：Test sample is put in the dry test tube of tool plug, the preparation method of sighting target directrix curve " is waved in water-bath certainly
Dry solvent " rises, and measures absorbance in accordance with the law, and the amount of ruscogenin in calibration set sample is read from standard curve, calculates, i.e.,
.
4. the measure of calibration set sample Methylophiopogonanone A B and methylophiopogonanone B content
Methyl Radix Ophiopogonis in calibration set sample is measured using high performance liquid chromatography and UV detector combination method (HPLC-UV methods)
The content of Homoisoflavonoids A and methylophiopogonanone B；
(1) analysis condition：Chromatographic column is Agilent Zorbax C18 (4.6mm × 250mm, 5 μm), and mobile phase is second
The phosphoric acid solution of nitrile -0.1% (58: 42), flow velocity 1.0mL/min, 30 DEG C of column temperature, sampling volume 10 μ L, Detection wavelength 280nm；
(2) preparation of standard items：Precision weighs two reference substances respectively, adds methanol that every 1mL Radix Ophiopogonis containing methyl dihydro is made
The mixed reference substance solution of 33.8 μ g/mL of 20.4 μ g/mL of homoisoflavone A and methylophiopogonanone B to get；
(3) preparation of standard curve：By mixed reference substance solution respectively with 1 μ L, 2 μ L, 5 μ L, 10 μ L, 15 μ L, 20 μ L into
Sample carries out linear regression with sample size m (μ g) to chromatographic peak area A, draws the standard curve of two compounds, standard curve letter
Breath is as shown in table 2.
Regression analysis standard curve, related coefficient and the range of linearity of 2 homoisoflavone of table
(4) Methylophiopogonanone A B and methylophiopogonanone B assay：Calibration set sample is taken,
After 0.45 μm of filtering with microporous membrane, subsequent filtrate is taken to inject liquid chromatograph, by external standard method with two compounds of calculated by peak area
Content, as reference data.
5. calibration set sample spectrum data acquire
The calibration set sample being collected into is diluted ten times with pure water, uses ultraviolet-visible spectrophotometer (Cary60, U.S.
Agilent companies of state) scanning obtain the ultraviolet full spectrum of wavelengths of calibration samples collection 190~800nm ranges；It is molten by blank of water
Liquid, each sample make 3 parallel sweeps, take ultraviolet-visible characteristic absorption spectrum data of the average spectroscopic data as sample.It adopts
Mode set is transmission beam method, quartz colorimetric utensil of the cuvette used for light path 10mm, scanning accuracy 1nm.Collected sample set
Radix Ophiopogonis extract primary light spectrogram is referring to Fig. 2.
6. the foundation of calibration model
Initial data is handled using software for calculation BWIQTM softwares (U.S. B＆W Tek Opto-Electronics), to light
Spectrum carries out preprocess method and waveband selection optimization, is obtained with optimal wavelength band and sample preprocessing method processing initial data
To Radix Ophiopogonis alcohol extract characteristic spectrum information.The Quantifying model of 6 quality index is established using PCR methods, using leaving-one method
Intersect and carry out internal verification.
(1) different preprocessing procedures modeling optimizations：Respectively with SG is smooth, first derivative, second dervative pretreatment side
The full wave ultraviolet original spectrum of method processing, PCR method modelings are carried out by taking the numerical value of dwarf lilyturf tuber total saponins as an example, the results are shown in Table 3.With phase
Close coefficients R2, judgment basis of the root-mean-square error RMSE as model robustness, the results showed that at smooth and first derivative
Model performance after reason is best, i.e. related coefficient highest (R2=0.888), root-mean-square error (RMSE=1.882 μ g/mL) is most
It is small.Through SG is smooth and first derivative treated spectrogram is referring to Fig. 2.
The different preprocessing procedures PCR methods of table 3 establish dwarf lilyturf tuber total saponins model optimization result
(2) different-waveband spectroscopic data modeling optimization：Respectively with sample set all-wave length, 190-350nm, 190-450nm,
Tetra- wave bands of 190-600nm carry out PCR method modelings, the results are shown in Table 4.The result shows that：Select what this wave band of 190-450nm was established
Dwarf lilyturf tuber total saponins quantitative model performance is best, i.e. related coefficient (R2=0.969) highest, root-mean-square error (RMSE=0.987 μ
G/mL it is) minimum.
4 different-waveband range of table carries out PCR methods and establishes dwarf lilyturf tuber total saponins prediction model optimum results
(3) calibration model is established：SG exponential smoothing cunnings are carried out to the sample set ultra-violet absorption spectrum data of 190-450nm wave bands
And First derivative spectrograply pretreatment, establish the correction between Radix Ophiopogonis extract characteristic spectrum information and 6 quality index using PCR methods
Model is verified using leaving-one method internal chiasma.The related coefficient and cross validation error root mean square of 6 quantitative calibration models
RMSECV values are as shown in table 5.
6 quality index PCR regression model quantitative results of table 5 Radix Ophiopogonis alcohol extract sample set
There are preferable correlations between Radix Ophiopogonis extract characteristic spectrum and 6 quality index.With the quantitative calibration models
Correlativity figure between the reference point that 6 quality index contents of Radix Ophiopogonis extract and conventional method of prediction measure, is shown in Fig. 4 extremely
Fig. 9, wherein dwarf lilyturf tuber total saponins, Methylophiopogonanone A B, methylophiopogonanone B, fructose, glucose, sugarcane
Sugared content Quantifying model figure is followed successively by Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, and model above prediction is understood by Fig. 4 to Fig. 9
Value is good with correlation between reference point, and model has preferable performance.
7. the verification of calibration model
(each component content needs are fallen to be contained 3 Radix Ophiopogonis extracts that selection quality index has predicted in the corresponding ingredient of calibration set
Within the scope of amount) as verification collection, carry out ultra-violet absorption spectrum scanning by the identical ultraviolet spectra acquisition method of calibration set.Carry out phase
After same Pretreated spectra, spectrum characteristic parameter is inputted into calibration model, verification collection sample quality index content is calculated.This is pre-
Measured data the results are shown in Table 6 compared with reference point.
Predicted value, reference point and the RMSEP values of table 6PCR methods 6 quality index quantitative calibration models of Radix Ophiopogonis extract
Dwarf lilyturf tuber total saponins, Methylophiopogonanone A B, methylophiopogonanone B, fructose, glucose, sugarcane
The prediction error mean square root RMSEP of sugared content predicted value and reference point is acceptable prediction error.
8. the measure of each quality index of Shenmai injection production process Radix Ophiopogonis alcohol reflux extraction unit
Radix Ophiopogonis alcohol reflux extraction unit intermediate in big certain batch of production of Shenmai injection is taken, it is identical by calibration set sample
Ultraviolet spectra acquisition method collecting sample ultra-violet absorption spectrum data, by identical Pretreated spectra, input characteristic spectrum
The content value of corrresponding quality index in extracting solution can be quickly calculated in quantitative calibration models.6 obtained by calibration model
The content value of a quality index is as follows：Dwarf lilyturf tuber total saponins are 10.28 μ g/mL, Methylophiopogonanone A B is 0.0131 μ
G/mL, methylophiopogonanone B are 0.0109 μ g/mL, fructose is 6037 μ g/mL, glucose is 921 μ g/mL, sucrose
For 508 μ g/mL.The actual comparison measured with HPLC, difference is little, and spectrum rapid detection method is verified as reliably.
Embodiment 2：
According to the method for embodiment 1, difference part is to use software for calculation Simca-P+12.0 (Sweden Umetrics public affairs instead
Department), the quantitative calibration models of 6 quality index in Radix Ophiopogonis alcohol extract are established using PLS methods.
1. use calibration set sample and its reference point, ultraviolet spectra same as Example 1.
2. the foundation of calibration model
Initial data is handled using Simca, preprocess method is carried out to spectrum and waveband selection optimizes, with optimal wave band
Range and sample preprocessing method processing initial data obtain Radix Ophiopogonis alcohol extract characteristic spectrum information.6 matter are established using PLS methods
The Quantifying model of figureofmerit is intersected using leaving-one method and carries out internal verification.
(1) different preprocessing procedures modeling optimizations：Respectively with SG is smooth, first derivative, second dervative pretreatment side
The full wave ultraviolet original spectrum of method processing, PLS method modelings are carried out by taking the numerical value of dwarf lilyturf tuber total saponins as an example, the results are shown in Table 7.With
R2, judgment basis of the RMSE as model robustness, the results showed that using smooth and second dervative treated model performance most
It is good, i.e. related coefficient highest (R2=0.997), cross validation error root mean square (RMSECV=2.11 μ g/mL) is smaller.It is put down through SG
Sliding and second dervative treated spectrogram is referring to Figure 10.
The different preprocessing procedures PLS methods of table 7 establish dwarf lilyturf tuber total saponins model optimization result
(2) different-waveband spectroscopic data modeling optimization：Respectively with sample set all-wave length, 190-350nm, 190-450nm,
Tetra- wave bands of 190-600nm carry out PLS method modelings, the results are shown in Table 8.Comprehensive consideration R2After RMSECV, R is selected2Highest 190-
600nm wave bands are as modeling wave band.
8 different-waveband range of table carries out PLS methods and establishes dwarf lilyturf tuber total saponins prediction model optimum results
(3) calibration model is established：It is smooth and one that the sample set ultra-violet absorption spectrum data of 190-600nm wave bands are carried out with SG
Order derivative method pre-processes, and the straightening die between Radix Ophiopogonis extract characteristic spectrum information and 6 quality index is established using PLS methods
Type is verified using leaving-one method internal chiasma.The related coefficient and cross validation error root mean square of 6 quantitative calibration models
RMSECV values are as shown in table 9.
Six quality index PLS regression model quantitative results of table 9 Radix Ophiopogonis alcohol extract sample set
There are preferable correlations between Radix Ophiopogonis extract characteristic spectrum and 6 quality index.With the quantitative calibration models
Correlativity figure between the reference point that 6 quality index contents of Radix Ophiopogonis extract and conventional method of prediction measure, is shown in Figure 11
To Figure 16, wherein dwarf lilyturf tuber total saponins, Methylophiopogonanone A B, methylophiopogonanone B, fructose, grape
Sugar, cane sugar content Quantifying model figure are followed successively by Figure 11, Figure 12, Figure 13, Figure 14, Figure 15, Figure 16, from Figure 11 to Figure 16
Correlation is good between model above predicted value and reference point, and model has preferable performance.
3. the verification of calibration model
(each component content needs are fallen to be contained 3 Radix Ophiopogonis extracts that selection quality index has predicted in the corresponding ingredient of calibration set
Within the scope of amount) as verification collection, carry out ultra-violet absorption spectrum scanning by the identical ultraviolet spectra acquisition method of calibration set.Carry out phase
After same Pretreated spectra, spectrum characteristic parameter is inputted into calibration model, verification collection sample quality index content is calculated.This is pre-
Measured data the results are shown in Table 10 compared with reference point.
Predicted value, measured value and the RMSEP values of table 10PLS methods six quality index quantitative calibration models of Radix Ophiopogonis extract
Dwarf lilyturf tuber total saponins, Methylophiopogonanone A B, methylophiopogonanone B, fructose, glucose, sugarcane
The correlativity figure of sugared content predicted value and reference point is shown in Figure 17, Figure 18, Figure 19, Figure 20, Figure 21 and Figure 22, Radix Ophiopogonis total soap respectively
Glycosides, Methylophiopogonanone A B, methylophiopogonanone B, fructose, glucose, cane sugar content predicted value and ginseng
Prediction error mean square root RMSEP according to value is acceptable prediction error.
4. the measure of each quality index of Shenmai injection production process Radix Ophiopogonis alcohol reflux extraction unit
Radix Ophiopogonis alcohol reflux extraction unit intermediate in big certain batch of production of Shenmai injection is taken, it is identical by calibration set sample
Ultraviolet spectra acquisition method collecting sample ultra-violet absorption spectrum data, by identical Pretreated spectra, input characteristic spectrum
The content value of corrresponding quality index in extracting solution can be quickly calculated in quantitative calibration models.6 obtained by calibration model
The content value of a quality index is as follows：Dwarf lilyturf tuber total saponins are 10.59 μ g/mL, Methylophiopogonanone A B is 0.0140 μ
G/mL, methylophiopogonanone B are 0.0112 μ g/mL, fructose is 6087 μ g/mL, glucose is 946 μ g/mL, sucrose
For 504 μ g/mL.The actual comparison measured with HPLC, difference is little, and spectrum rapid detection method is verified as reliably.
Claims (3)
1. a kind of method of 6 quality index content of material in quick detection Radix Ophiopogonis alcohol extract, 6 quality index substances
For fructose, glucose, sucrose, dwarf lilyturf tuber total saponins, Methylophiopogonanone A B and methylophiopogonanone B,
It is characterized in that, this method includes the following steps：
(1) calibration set sample is collected：The Radix Ophiopogonis of different batches is selected, is collected in the different phase of Radix Ophiopogonis alcohol reflux extraction process
Radix Ophiopogonis alcohol extract is as calibration set sample；
(2) 6 quality index substance reference points of calibration set sample measure：A, using high performance liquid chromatography and Evaporative light scattering detector
Device combination method measures the content of fructose, dextrose and saccharose；B, using the content of perchloric acid determination of color dwarf lilyturf tuber total saponins；c、
Methylophiopogonanone A B and methylophiopogonanone B are measured using high performance liquid chromatography-ultraviolet light detection method
Content；
(3) measure of calibration set sample ultra-violet absorption spectrum：Using the quartz colorimetric utensil of light path 10mm, calibration set sample is diluted
Liquid, which is placed in ultraviolet-visual spectrometer, carries out full wavelength scanner, wavelength scanning range be 190~800nm, scanning accuracy 1nm,
Using water as blank solution, each sample makees 3 parallel sweeps, takes ultraviolet-visible absorption spectroscopy of the average spectroscopic data as sample
Data obtain calibration set sample ultraviolet-visible absorption spectroscopy data；
(4) calibration model is established：Using multivariate data analysis method, 6 quality index content of material in calibration set sample are established
The mathematical model of relationship between corresponding ultraviolet-visible absorption spectroscopy, related coefficient >=0.9 of the calibration model；
(5) calibration model is verified：The calibration model that step (4) is established using leaving-one method is intersected and carries out internal verification, verification
Method be to take Radix Ophiopogonis alcohol extract to be measured, measure its ultraviolet-visible absorption spectroscopy, be inputted the school of each quality index substance
In positive model, the content of corrresponding quality index substance in calculating is measured with the Radix Ophiopogonis alcohol extract according to step (2) method each
Quality index content of material compares, it is desirable that measurement error is less than or equal to 25%；
(6) 6 quality index content of material of Radix Ophiopogonis alcohol extract to be measured are calculated：Take 6 quality index content of material to be measured
Winter wheat extracting solution sample, according to the ultravioletvisible absorption light of the ultraviolet spectra acquisition method collecting sample identical with calibration set sample
Spectrum information inputs the spectral information in the calibration model of each quality index substance, calculates corrresponding quality index in sample to be tested
The content of substance.
2. the method for 6 quality index content of material in a kind of quick detection Radix Ophiopogonis alcohol extract as described in claim 1,
It is characterized in that, the multivariate data analysis method described in step (4) is principal component regression method or Partial Least Squares.
3. the method for 6 quality index content of material exists in a kind of quick detection Radix Ophiopogonis alcohol extract as described in claim 1
Answering during 6 quality index content of material measure in Radix Ophiopogonis alcohol extracting unit intermediate is measured in Shenmai injection production process
With.
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| CN109541098A (en) * | 2018-11-27 | 2019-03-29 | 华润三九（雅安）药业有限公司 | Radix Ophiopogonis finger-print, its construction method and Radix Ophiopogonis quality determining method |
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