成分分析

HPLC法同时测定复方利血平片中7个成分的含量*

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  • 上海市食品药品检验研究院 国家药品监督管理局化学药品制剂质量分析重点实验室,上海 201203
第一作者 Tel:13788965965;E-mail:qianmin@smda.sh.cn
** Tel:(021)50798193;E-mail:fdalej@163.com

收稿日期: 2021-08-12

  网络出版日期: 2024-06-24

基金资助

* 国家药典委员会药品标准制修订研究课题(2019H064)

Simultaneous determination of the content of seven components in compound reserpine tablets by HPLC*

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  • Shanghai Institute for Food and Drug Control, National Medical Products Administration Key Laboratory for Quality Analysis of Chemical Drug Preparations, Shanghai 201203, China

Received date: 2021-08-12

  Online published: 2024-06-24

摘要

目的:建立HPLC法同时测定复方利血平片中利血平、氢氯噻嗪、硫酸双肼屈嗪、盐酸异丙嗪、维生素B1、维生素B6和泛酸钙7个成分的含量。方法:采用Agilent Zorbax SB-C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈(A)-0.03 mol·L-1磷酸二氢钾溶液(含0.25%庚烷磺酸钠,用磷酸调节pH至4.0)(B)为流动相,梯度洗脱(0~7 min,5%A→18%A;7~15 min,18%A;15.1~23 min,50%A;23.1~30 min,5%A),流速1.0 mL·min-1,柱温40 ℃,检测波长205 nm(0~7 min,泛酸钙)、275 nm(7~17 min,氢氯噻嗪、维生素B6、硫酸双肼屈嗪和维生素B1)、215 nm(17~30 min,盐酸异丙嗪和利血平),进样体积20 μL。结果:利血平、氢氯噻嗪、硫酸双肼屈嗪、盐酸异丙嗪、维生素B1、维生素B6和泛酸钙的浓度在相应的范围内与峰面积呈良好线性关系(r均>0.999);低、中、高3个浓度水平9份样品的平均加样回收率分别为99.8%(RSD=1.4%)、98.9%(RSD=1.5%)、100.4%(RSD=1.4%)、99.8%(RSD=1.0%)、99.2%(RSD=1.2%)、100.9%(RSD=1.1%)、100.2%(RSD=1.2%);精密度、稳定性良好,RSD均<2.0%。薄膜衣片(6个生产企业共17个批次)中7个成分的含量均介于标示量的93.0%~108.2%;糖衣片(1个生产企业共3个批次)中7个成分的含量均介于标示量的75.2%~108.0%。结论:该方法简便快捷,专属性好,可用于复方利血平片的质量控制,为质量标准提高提供参考。

本文引用格式

钱敏, 宋冬梅, 凌霞, 乐健 . HPLC法同时测定复方利血平片中7个成分的含量*[J]. 药物分析杂志, 2022 , 42(7) : 1110 -1119 . DOI: 10.16155/j.0254-1793.2022.07.02

Abstract

Objective: To establish an HPLC method for the simultaneous determination of reserpine, hydrochlorothiazide, dihydralazine sulfate, promethazine hydrochloride, vitamin B1, vitamin B6 and calcium pantothenate in compound reserpine tablets. Methods: HPLC experiment was performed on an column of Agilent Zorbax SB-C18(250 mm×4.6 mm,5 μm) with the mobile phase of acetonitrile(A)-0.03 mol·L-1 KH2PO4(containing 0.25% of heptanesulfonic acid sodium and adjust pH to 4.0 with phosphoric acid)(B) with gradient elution (0-7 min, 5%A→18%A; 7-15 min, 18%A; 15.1-23 min, 50%A; 23.1-30 min, 5%A). The flow rate was 1.0 mL·min-1, the column temperature was 40 ℃, and the detection wavelength was 205 nm(0-7 min for calcium pantothenate), 275 nm(7-17 min for hydrochlorothiazide, vitamin B6, dihydralazine sulfate, vitamin B1) and 215 nm(17-30 min for promethazine hydrochloride and reserpine). The injection volume was 20 μL. Results: Reserpine, hydrochlorothiazide, dihydralazine sulfate, promethazine hydrochloride, vitamin B1, vitamin B6 and calcium pantothenate showed good linear relationships with the peak area in the corresponding range (r>0.999), the average recoveries of 9 samples at low, medium and high concentration levels were 99.8% (RSD=1.4%), 98.9%(RSD=1.5%), 100.4%(RSD=1.4%), 99.8%(RSD=1.0%), 99.2%(RSD=1.2%), 100.9%(RSD=1.1%), 100.2%(RSD=1.2%) respectively. The precision and stability were good with RSDs less than 2%. The contents of 7 components in film-coated tablets(6 manufacturing enterprises, a total of 17 batches) were between 93.0% and 108.2% of the labeled amount. The contents of 7 ingredients in sugar-coated tablets were between 75.2% and 108.0% of the marked amount. Conclusion: The established method is simple, rapid, specific for the quality control of compound reserpine tablets. It provides reference for improving the quality standards of compound reserpine tablets.

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