超高效液相色谱法测定复方罗布麻片Ⅰ化学药成分方法的建立与确证  

Establishment and Confirmation of a Method for the Determination of Chemical Components in Compound Apocynum Tablets Ⅰ by Ultra High Performance Liquid Chromatography

作　　者：刘晓强 张岩琛 刘旻虹 张晓栋 王玲娜 LIU Xiao-Qiang;ZHANG Yan-Chen;LIU Min-Hong;ZHANG Xiao-Dong;WANG Ling-Na(Changzhou Food and Drug Supervision and inspection Center,Changzhou 213001 China)

机构地区：[1]常州市食品药品监督检验中心,江苏常州213001

出　　处：《中国药物经济学》2020年第7期53-59,共7页China Journal of Pharmaceutical Economics

基　　金：江苏省食品药品监督管理局科研项目(技术类项目)(20170219)。

摘　　要：目的建立并验证复方罗布麻片Ⅰ化学药成分超高效液相色谱法(UPLC)测定方法。方法采用Waters ACQUITY H-ClassCYANO(3.0×100mm,1.8μm),以0.07%的己烷磺酸钠溶液(用磷酸调节pH值至2.75)为流动相A,甲醇:乙腈=5:1为流动相B进行梯度洗脱,流速为0.53 ml/min,柱温30℃。检测波长为275、250 nm,稀释溶剂为0.1 mol/L盐酸。结果硫酸双肼嗪线性范围为38.4~153.6μg/ml,r=0.9998;氢氯噻嗪线性范围为38.4~153.6μg/ml,r=0.9999;盐酸异丙嗪线性范围为25.2~100.8μg/ml,r=0.9998;维生素B1线性范围为12~48μg/ml,r=0.9999;维生素B6线性范围12~48μg/ml,r=0.9998。各组分精密度良好,且无明显膜吸附,除硫酸双肼屈嗪外,提取回收率良好。结论该方法可用于测定和评估市售复方罗布麻片Ⅰ化学药成分含量。Objective To establish and verify UP/LC method for determination of chemical constituents in compound Apocynum venetum Tablets Ⅰ. Methods A Waters ACQUITY H-Class CYANO(1.8 um 3.0×100 mm) was used, with gradient elution of 0.07% sodium hexane sulfonate solution(adjusting pH value to 2.75 with phosphoric acid) as mobile phase A and Methanol: acetonitrile = 5:1 as mobile phase B at a flow rate of 0.53 m L·min-1. The detection wavelength was set at 275 and 250 nm. The column temperature was 30 ℃. The dilution solvent was 0.1 mol·L-1 hydrochloric acid. Results The linear range of dihydrazine sulfate was 38.4-153.6 μg·ml-1, r=0.9998, hydrochlorothiazide was 38.4-153.6 μg·ml-1, r=0.9999, promethazine hydrochloride was 25.2-100.8 μg·ml-1, r=0.9998, vitamin B1 was 12-48 μg·ml-1, r=0.9999, vitamin B6 is 12-48 μg·ml-1, r=0.9998. The precision of each groups was good, and there was no obvious membrane adsorption. Except dihydrazine sulfate, the recovery rate was good. Conclusion The method can be used for the determination and evaluation of chemical constituents in compound Apocynum Tablets Ⅰ.

关 键 词：超高效液相色谱法 复方罗布麻片Ⅰ 硫酸双肼屈嗪 中药浸膏 生产工艺 

分 类 号：R917[医药卫生—药物分析学]