小儿咽扁颗粒中掺伪山银花检验方法研究

姜军华; 吴良发; 许妍; 戴忠; 周志强

文章摘要

姜军华,吴良发,许妍,戴忠,周志强.小儿咽扁颗粒中掺伪山银花检验方法研究[J].中国药事,2023,(4):443-449

小儿咽扁颗粒中掺伪山银花检验方法研究

Study on the Test Method of Adulterated Lonicerae Flos in Xiaoer Yanbian Granule

DOI：10.16153/j.1002-7777.2023.04.011

中文关键词: 小儿咽扁颗粒金银花山银花灰毡毛忍冬皂苷乙高效液相色谱-蒸发光散射检测器法

英文关键词: Xiaoer Yanbian Granule Lonicerae Japonicae Flos Lonicerae Flos Macranthoidin B HPLC-ELSD

基金项目:江西省药品监督管理局科研项目(编号 2019JS05)

作者	单位
姜军华	江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌 330029
吴良发	江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌 330029
许妍	江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌 330029
戴忠	中国食品药品检定研究院,北京 100050
周志强	江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌 330029

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中文摘要:

目的：建立小儿咽扁颗粒中山银花的高效液相色谱-蒸发光散射检测器(HPLC-ELSD)检查方法，打击中药制剂中金银花的掺假行为。方法：采用薄层色谱(TLC)法，以灰毡毛忍冬皂苷乙为指标成分，以三氯甲烷-甲醇-水(6∶4∶1)为展开剂，快速筛查小儿咽扁颗粒中掺伪的山银花；采用HPLC-ELSD法鉴别小儿咽扁颗粒中掺伪的山银花，选择Sun Fire^® C₁₈(4.6 mm×250 mm，5 μm)色谱柱，流动相为乙腈-水，梯度洗脱，流速1 mL·min^-1，柱温 30 ℃，进样量 10 μL；采用高效液相色谱-串联质谱(HPLC-MS)法进行确证，选择Thermo Hypersil GOLD aQ C18(150 mm×2.1 mm， 3 μm)色谱柱，以乙腈-0.1%甲酸溶液为流动相梯度洗脱，流速0.3 mL·min-1，柱温30 ℃，质谱使用电喷雾离子源，负离子模式下检测。结果：TLC法检测结果显示，34批样品中共有8家企业生产的16批次样品疑似检出灰毡毛忍冬皂苷乙；HPLC-ELSD法的验证结果与TLC法一致，小儿咽扁颗粒中金银花掺伪山银花5%及以上即可检出；16批次检出灰毡毛忍冬皂苷乙样品均得到HPLC-MS法确证。结论：所建系列方法专属性好，灵敏度高，简便、快捷，为打击金银花掺伪提供了有力的技术支撑。

英文摘要:

Objective: To establish the HPLC-ELSD identifi cation method of Lonicerae Flos in Xiaoer Yanbian granules, crack down on the adulteration of Lonicerae Japonicae Flos in traditional Chinese medicine preparations. Methods: The adulterated Lonicerae Flos in Xiaoer Yanbian granules were quickly screen by TLC with macranthoidin B as the index component and trichloromethane methanol water (6∶4∶1) as the developing agent; The adulterated Lonicerae Flos in Xiaoer Yanbian granules were identifi ed by HPLC-ELSD, a Sun Fire^® C₁₈(2) column (4.6 mm × 250 mm, 5μm) was selected, the mobile phase was acetonitrile-water with gradient elution, the fl ow rate was 1.0 mL·min^-1, the column temperature was 30 ℃, and the sample volume was 10 μL; it was confi rmed by LC-MS, and the column was Thermo Hypersil GOLD aQ C₁₈ (150 mm ×2.1 mm, 3 μm) gradiently eluted with acetonitrile-0.1% formic acid solution as the mobile phase at the fl ow rate of 0.3 mL·min^-1, and the column temperature was 30 ℃. Electrospray ion source was used for mass spectrometer, detected in negative ion mode. Results: TLC test results showed that a total of 16 batches of 34 samples produced by 8 enterprises were suspected of detecting macranthoidin B; the verifi cation result of HPLC-ELSD method were consistent with TLC method, and 5% or more of Lonicerae Flos mixed with Lonicerae Japonicae Flos in Xiaoer Yanbian granules could be detected. The 16 batches of macranthoidin B samples were confi rmed by HPLC-MS. Conclusion: The established series of methods have good specificity, high sensitivity, simplicity and rapidity, and it provides a strong technical support for combating Lonicerae Japonicae Flos adulteration.

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