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    L-Lysine HCL

    Uploaded by

    Muhammad Zubair
    The document describes specifications and testing methods for L-Lysine Hydrochloride drug substance. It lists 7 specifications including description, solubility, identification, optical rotation, loss on drying, chloride content, and assay. 11 analytical tests are also described covering appearance, solubility, identification by spectroscopy, optical rotation, loss on drying, chloride content via titration, residue on ignition, related impurities via TLC, iron content, and assay via titration to determine percentage of L-Lysine Hydrochloride. Acceptance criteria are provided for each test to ensure the drug substance meets pharmacopeial standards.

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    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd

    L-Lysine HCL

    Uploaded by

    Muhammad Zubair
    82 views4 pages
    The document describes specifications and testing methods for L-Lysine Hydrochloride drug substance. It lists 7 specifications including description, solubility, identification, optical rotation, loss on drying, chloride content, and assay. 11 analytical tests are also described covering appearance, solubility, identification by spectroscopy, optical rotation, loss on drying, chloride content via titration, residue on ignition, related impurities via TLC, iron content, and assay via titration to determine percentage of L-Lysine Hydrochloride. Acceptance criteria are provided for each test to ensure the drug substance meets pharmacopeial standards.

    Original Description:

    Lysine Testing specification

    Original Title

    L-Lysine HCl

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    The document describes specifications and testing methods for L-Lysine Hydrochloride drug substance. It lists 7 specifications including description, solubility, identification, optical rotation, loss on drying, chloride content, and assay. 11 analytical tests are also described covering appearance, solubility, identification by spectroscopy, optical rotation, loss on drying, chloride content via titration, residue on ignition, related impurities via TLC, iron content, and assay via titration to determine percentage of L-Lysine Hydrochloride. Acceptance criteria are provided for each test to ensure the drug substance meets pharmacopeial standards.

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    82 views4 pages

    L-Lysine HCL

    Uploaded by

    Muhammad Zubair
    The document describes specifications and testing methods for L-Lysine Hydrochloride drug substance. It lists 7 specifications including description, solubility, identification, optical rotation, loss on drying, chloride content, and assay. 11 analytical tests are also described covering appearance, solubility, identification by spectroscopy, optical rotation, loss on drying, chloride content via titration, residue on ignition, related impurities via TLC, iron content, and assay via titration to determine percentage of L-Lysine Hydrochloride. Acceptance criteria are provided for each test to ensure the drug substance meets pharmacopeial standards.

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    © All Rights Reserved
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    Specifications and Testing Method of L-Lysine Hydrochloride Drug Substance

    Sr.
    No Parameters Acceptance Criteria/Limits Specification
    .
    1.0 Description White, odorless powder

    2.0 Solubility . Freely soluble in water

    3.0 Identification Must be positive Lysine Hydrochloride

    4.0 Optical Rotation +20.4° to +21.4° USP

    5.0 Loss on Drying NMT 0.4%

    Content of
    6.0 9.0%–19.6%
    Chloride

    Lysine Hydrochloride contains NLT 98.5% and


    7.0 Assay NMT 101.5% of L-lysine hydrochloride calculated
    on the dried basis.
    Specifications and Testing Method of L-Lysine Hydrochloride Drug Substance

    A1 Appearance:
    White, odorless powder

    A2 Solubility:
    Freely soluble in water

    A3 Identification:
    The spectrum of sample solution must be concordant with that of standard solution

    A4 Optical Rotation:
    +20.4° to +21.4°, measured at 25 ºC.
    Sample solution: 80 mg/mL in 6 N hydrochloric acid.

    A5 Loss on Drying
    Dry a sample at 105° for 3 h: it loses
    NMT 0.4% of its weight.

    A6 Content Of Chloride
    Sample: 350 mg of Lysine Hydrochloride
    Blank: 140 mL of water
    Titrimetric system
    Mode: Direct titration
    Titrant: 0.1 N silver nitrate VS
    Endpoint detection: Visual
    Analysis: Transfer the Sample to a porcelain casserole, and add 140 mL of water and 1
    mL of dichlorofluorescein TS.
    Titrate with the Titrant until the silver chloride flocculates and the mixture acquires a faint
    pink color. Perform the
    Blank determination.
    Calculate the percentage of chloride (Cl) in the Sample taken:

    Result = {[(V S − V B) × N × F]/W} × 100


    V S = Titrant volume consumed by the Sample (mL)
    V B = Titrant volume consumed by the Blank (mL)
    N = actual normality of the Titrant (mEq/mL)
    F = equivalency factor, 35.45 mg/mEq
    W = Sample weight (mg)
    Acceptance criteria: 19.0%–19.6%

    A7 Residue On Ignition:
    NMT 0.1%

    A8 Chloride And Sulfate, Sulfate


    Standard solution: 0.10 mL of 0.020 N sulfuric acid
    Sample: 0.33 g of Lysine Hydrochloride
    Acceptance criteria: NMT 0.03%
    Specifications and Testing Method of L-Lysine Hydrochloride Drug Substance

    A9 Iron
    NMT 30 ppm
    A10 Related Compounds
    Standard solution: 0.05 mg/mL of USP L-Lysine
    Hydrochloride RS in water. [NOTE—This solution has a concentration equivalent to
    0.5% of that of the Sample solution.]
    Sample solution: 10 mg/mL of Lysine Hydrochloride in water
    System suitability solution: 0.4 mg/mL each of USP
    L-Lysine Hydrochloride RS and USP Arginine
    Hydrochloride RS
    Chromatographic system
    Mode: TLC
    Adsorbent: 0.25-mm layer of chromatographic silica gel mixture
    Application volume: 5 μL
    Developing solvent system: Isopropyl alcohol and ammonium hydroxide (7:3)
    Spray reagent: 0.2 g of ninhydrin in a mixture of butyl alcohol and 2 N acetic acid (95:5)
    System suitability
    Suitability requirements: The chromatogram of the
    System suitability solution exhibits two clearly separated spots.
    Analysis
    Samples: Standard solution, System suitability solution, and Sample solution
    Dry the plate between 100° and 105° until the ammonia
    completely disappears. Spray with Spray reagent, and
    heat between 100° and 105° for 15 min. Examine the
    plate under white light.
    Acceptance criteria: Any secondary spot of the Sample
    solution is not larger or more intense than the principal spot
    of the Standard solution.
    Individual impurities: NMT 0.5%
    Total impurities: NMT 2.0%

    A11 Assay
    Sample: 90 mg of Lysine Hydrochloride
    Blank: Mix 3 mL of formic acid and 50 mL of glacial acetic acid.
    Titrimetric system
    Mode: Direct titration
    Titrant: 0.1 N perchloric acid VS
    Endpoint detection: Potentiometric
    Analysis: Dissolve the Sample in 3 mL of formic acid and 50 mL of glacial acetic acid.
    Add 10 mL of mercuric acetate TS, and titrate with the Titrant. Perform the Blank
    determination.
    Calculate the percentage of lysine hydrochloride
    (C6H14N2O2 · HCl) in the Sample taken:
    Result = {[(V S − V B) × N × F]/W} × 100
    V S = Titrant volume consumed by the Sample (mL)
    V B = Titrant volume consumed by the Blank (mL)
    N = actual normality of the Titrant (mEq/mL)
    F = equivalency factor, 91.33 mg/mEq
    Specifications and Testing Method of L-Lysine Hydrochloride Drug Substance

    W = Sample weight (mg)


    Acceptance criteria: 98.5%–101.5% on the dried basis

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