HPLC法同时测定复方利血平片中7个成分的含量  

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

作　　者：钱敏 宋冬梅 凌霞 乐健 QIAN Min;SONG Dong-mei;LING Xia;LE Jian(Shanghai Institute for Food and Drug Control.,National Medical Products Administration Key Laboratory for Quality Analysis of Chemical Drug Preparations,Shanghai 201203,China)

机构地区：[1]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

出　　处：《药物分析杂志》2022年第7期1110-1119,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委员会药品标准制修订研究课题(2019H064)。

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B_(1)、维生素B_(6)和泛酸钙7个成分的含量。方法:采用Agilent Zorbax SB-C_(18)色谱柱(250 mm×4.6 mm,5μm),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B_(6)、硫酸双肼屈嗪和维生素B_(1))、215 nm(17~30 min,盐酸异丙嗪和利血平),进样体积20μL。结果:利血平、氢氯噻嗪、硫酸双肼屈嗪、盐酸异丙嗪、维生素B_(1)、维生素B_(6)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。Objective:To establish an HPLC method for the simultaneous determination of reserpine,hydrochlorothiazide,dihydralazine sulfate,promethazine hydrochloride,vitamin B_(1),vitamin B_(6) and calcium pantothenate in compound reserpine tablets.Methods:HPLC experiment was performed on an column of Agilent Zorbax SB-C_(18)(250 mm×4.6 mm,5μm)with the mobile phase of acetonitrile(A)-0.03 mol·L^(-1) KH_(2)PO_(4)(containing0.25%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^(-1)5 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^(-1)7 min for hydrochlorothiazide,vitamin B_(6),dihydralazine sulfate,vitamin B_(1))and 215 nm(17-30 min for promethazine hydrochloride and reserpine).The injection volume was 20μL.Results:Reserpine,hydrochlorothiazide,dihydralazine sulfate,promethazine hydrochloride,vitamin B_(1),vitamin B_(6) 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.

关 键 词：复方利血平片 利血平 氢氯噻嗪 硫酸双肼屈嗪 盐酸异丙嗪 维生素 泛酸钙 高效液相色谱法 质量控制 

分 类 号：R917[医药卫生—药物分析学]