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离子对高效液相色谱法测定多库酯钠的含量

蔡立荣, 舒海平, 肖莎, 谭跃, 郑金凤, 李昌亮, 刘雁鸣

蔡立荣,舒海平,肖莎,等. 离子对高效液相色谱法测定多库酯钠的含量[J]. 中国药科大学学报,2025,56(2):183 − 187. DOI: 10.11665/j.issn.1000-5048.2024081002
引用本文: 蔡立荣,舒海平,肖莎,等. 离子对高效液相色谱法测定多库酯钠的含量[J]. 中国药科大学学报,2025,56(2):183 − 187. DOI: 10.11665/j.issn.1000-5048.2024081002
CAI Lirong, SHU Haiping, XIAO Sha, et al. Determination of docusate sodium by ion-pair high-performance liquid chromatography[J]. J China Pharm Univ, 2025, 56(2): 183 − 187. DOI: 10.11665/j.issn.1000-5048.2024081002
Citation: CAI Lirong, SHU Haiping, XIAO Sha, et al. Determination of docusate sodium by ion-pair high-performance liquid chromatography[J]. J China Pharm Univ, 2025, 56(2): 183 − 187. DOI: 10.11665/j.issn.1000-5048.2024081002

离子对高效液相色谱法测定多库酯钠的含量

基金项目: 湖南省自然科学基金科药联合基金项目(2023JJ60106);国家药监局药物制剂及辅料研究与评价重点实验室开放课题(PPE2023008)
详细信息
    通讯作者:

    蔡立荣: Tel:0731-89912568 E-mail:iamcailirong@163.com

    刘雁鸣: Tel:0731-82275838 E-mail:380852839@qq.com

  • 中图分类号: R917

Determination of docusate sodium by ion-pair high-performance liquid chromatography

Funds: This study was supported by the Hunan Provincial Natural Science Foundation of China(2023JJ60106)and the NMPA Key Laboratory for Research and Evaluation of Pharmaceutical Preparation and Excipients Foundation(PPE2023008)
  • 摘要:

    为降低对高载碳量色谱柱的依赖,优化并建立了多库酯钠含量测定的新型离子对高效液相色谱法(IP-HPLC)。采用四丙基氯化铵为离子对试剂,乙腈-10 mmol/L四丙基氯化铵水溶液(66∶34)为流动相,用0.1%磷酸溶液调pH至6.5,流速为1.5 mL/min,检测波长为214 nm,柱温为35 ℃,进样量为25 μL,外标法测定。结果表明该方法专属性良好,主峰拖尾因子为1.34;在0.02~0.40 mg/mL范围内线性关系良好,相关系数r=0.9999;重复性结果良好,加样回收率97.0%~98.2%(n=6);定量限为3.31 μg/mL;检测限为2.76 μg/mL。总体来看,新方法耐用性好、线性范围宽、灵敏度高,适合用于测定多库酯钠的含量。

    Abstract:

    To reduce the dependency on high-carbon-load chromatographic columns,a new method has been established for the determination of the content of docusate sodium using ion-pair high-performance liquid chromatography (IP-HPLC). Tetrapropylammonium chloride was used as the ion-pair reagent with a mobile phase, composition of acetonitrile:10 mmol/L tetrapropylammonium chloride solution = 66∶34, adjusting pH to 6.5 with 0.1% phosphoric acid solution,flow rate of 1.5 mL/min, detection wavelength of 214 nm,column temperature of 35 °C, and an injection volume of 25 μL,and quantified by an external standard method. The main peak of docusate sodium exhibited a tailing factor of 1.34. The method showed good linearity within the range of 0.02 mg/mL to 0.40 mg/mL, with a correlation coefficient (r) of 0.999 9. It also demonstrated good repeatability, with recovery ranging from 97.0% to 98.2% (n=6). The quantification limit was 3.31 μg/mL, and the detection limit was 2.76 μg/mL.In summary,the new method shows good durability, a wide linear range, and high sensitivity, it is suitable for the determination of docusate sodium.

  • Figure  1.   Chromatograms and retention behavior at different pH conditions

    A:pH 7.51; B:pH 6.48;C:pH 5.51;D:pH 4.50;E:pH 3.61

    Figure  2.   Reported ionic impurities in docusate sodium

    Figure  3.   Chromatographic performance results of the USP method in different loading columns(DS:Docusate sodium)

    A:Thermo Hypersil GOLD;B:GL Sciences ODS-3;C:Waters Symmetry C18;D:Phenomenex Ultracarb ODS(30)60 Å

    Figure  4.   Chromatographic performance results of the new method in different loading columns

    A:Thermo Hypersil GOLD; B:GLSciences ODS-3;C:Waters Symmetry C18;D:Phenomenex UltracarbODS(30)60 Å

    Table  1   Effect of ions pair type on the separation performance

    Ion pair type tR/min Peak area Plate number Symmetry factor
    Tetramethylammonium chloride 3.03 50050 643 1.49
    Tetraethylammonium chloride 4.65 45173 454 1.14
    Tetrapropylammonium chloride 5.21 47084 1637 1.50
    Tributylmethylammonium chloride 6.50 48425 2112 1.47
    Tetrabutylammonium chloride 7.40 57387 1585 1.18
    Tetrapentylammonium chloride 14.15 31807 2705 1.27
    下载: 导出CSV

    Table  2   Results of forced degradation testing

    Conditions Peak area ratio/%
    Main peak Impurity A Impurity B Impurity C Impurity D Others
    Untreated 98.08 1.76 / 0.16 / /
    High temperature 98.29 1.53 / 0.18 / /
    Light exposure 97.36 2.49 / 0.15 / /
    Strong acid 97.08 2.92 / / / /
    Strong alkali 86.01 13.99 / / / /
    Oxidation 96.16 3.84 / / / /
    /:Not detected
    下载: 导出CSV

    Table  3   HPLC results and titration results for samples from three manufacturers

    Manufacturer Batch No. New method ChP2020(1st Suppl.) method
    Main component Total impurity
    Domestic Company A 211106 96.8% 0.5% 97.2%
    Domestic Company B T202111YC02 92.7% 0.9% 94.8%
    Import Company A WS21F0803 95.6% 3.7% 97.5%
    下载: 导出CSV

    Table  4   Column type specifications

    No. Brand Type Carbon loading/%
    A Thermo Hypersil GOLD, 250 mm×4.6 mm,5 μm 10
    B GL Sciences ODS-3, 250 mm×4.6 mm,5 μm 15
    C Waters Symmetry C18, 250 mm×4.6 mm,5 μm 20
    D Phenomenex Ultracarb,150 mm×4.6 mm,5 μm 30
    下载: 导出CSV
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    [2]

    The United States Pharmacopeial Convention. USP-NF[S/OL]. Docusate sodium, 2018, [2023-08-01]. https://doi.org/10.31003/USPNF_M27920_03_01.

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    [6]

    The United States Pharmacopeial Convention,USP-NF[S/OL]. Docusate Sodium Capsules, 2013 [2023-08-01]. https://doi.org/10.31003/USPNF_M27930_01_01.1.

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图(4)  /  表(4)
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出版历程
  • 收稿日期:  2024-08-09
  • 刊出日期:  2025-04-24

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