复方小儿退热栓的质量标准提高研究  

Study on Quality Standard Improvement for Compound Child Antifebrile Suppository

作　　者：谢思敏[1] 陈家仪[1] 汤迎湛 顾利红[1] 栗建明[1] 侯惠婵[1] XIE Simin;CHEN Jiayi;TANG Yingzhan;GU Lihong;LI Jianming;HOU Huichan(Guangzhou Institute for Drug Control/Key Laboratory for Quality Evaluation of Chinese Patent Medicine,National Medical Products Administration,Guangzhou 510160,China;Guangzhou Baiyunshan Jingxiutang Phannaceutical Co.,Ltd.,Guangzhou 510130,China)

机构地区：[1]广州市药品检验所/国家药品监督管理局中成药质量评价重点实验室,广州510160 [2]广州白云山敬修堂药业股份有限公司,广州510130

出　　处：《中国药房》2020年第17期2106-2111,共6页China Pharmacy

基　　金：国家药典委员会药品标准制修订研究课题(NO.2019Z028)。

摘　　要：目的:提高复方小儿退热栓的药品质量标准。方法:在原质量标准的基础上,建立处方中人工牛黄和南板蓝根的薄层色谱(TLC)鉴定方法;建立胆酸、猪去氧胆酸、对乙酰氨基酚含量测定的高效液相色谱(HPLC)法。结果:复方小儿退热栓中人工牛黄和南板蓝根的TLC图谱均与相应的对照品或对照药材在相同位置上显现相同颜色的斑点,且相应的阴性样品无干扰。HPLC法采用色谱柱分别为Welch Xtimate C18柱(胆酸、猪去氧胆酸)、Agilent ZORBAX SB-C18柱(对乙酰氨基酚);流动相分别为乙腈-0.5%甲酸溶液(梯度洗脱,胆酸、猪去氧胆酸)、甲醇-水溶液(20∶80,V/V,对乙酰氨基酚);流速为1.0 mL/min;蒸发光散射检测器的漂移管温度为105℃,载气流速为2.0 L/min(胆酸、猪去氧胆酸);紫外检测波长为244 nm(对乙酰氨基酚)。胆酸、猪去氧胆酸、对乙酰氨基酚进样量分别在0.1500~4.5000、0.2125~6.3750、0.0819~1.6385μg范围内线性关系良好(r均大于0.9992);精密度、重复性、稳定性试验的RSD均小于3%(n=6或n=7);平均加样回收率分别为100.35%、101.39%、98.81%,RSD均小于3%(n=6)。结论:本研究在复方小儿退热栓原质量标准的基础上,增加了人工牛黄和南板蓝根的TLC鉴别方法,并采用HPLC法测定胆酸、猪去氧胆酸、对乙酰氨基酚的含量,能有效地提高该制剂的质量控制标准。OBJECTIVE:To improve the quality standard of Compound child antifebrile suppository.METHODS:Based on the previous quality standard,TLC identification methods were established for artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix.HPLC method was established for content determination of choleic acid(CA),hyodeoxycholic acid(HDCA)and paracetamol.RESULTS:TLC chromatogram of artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix all showed the same color spots in the same position as the corresponding substance control or reference medicinal material,while the negative samples had no interference.HPLC was performed on Welch Xtimate C18 column(CA,HDCA)or Agilent ZORBAX SB-C18 column(paracetamol)with mobile phase consisted of acetonitrile-0.5%formic acetic acid(by gradient elution,CA and HDCA)or methanol-water(20∶80,V/V,paracetamol)at the flow rate of 1.0 mL/min.ELSD was used with a nitrogen flow-rate of 2.0 L/min at a drift tube temperature of 105℃(CA,HDCA).The detection wavelength was set at 244 nm(paracetamol).The linear ranges of CA,HDCA,paracetamol were 0.1500-4.5000,0.2125-6.3750,0.0819-1.6385μg(all r>0.9992).RSDs of precision,reproducibility and stability tests were all lower than 3%(n=6 or n=7).The average recoveries were 100.35%,101.39%,98.81%(all RSD<3%,n=6).CONCLUSIONS:Based on previous quality standard of Compound child antifebrile suppository,TLC method is used to identify artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix,and the contents of CA,HDCA and paracetamol are determined by HPLC,which can effectively improve the quality control standard of the preparation.

关 键 词：复方小儿退热栓 薄层色谱 高效液相色谱法 鉴别 含量测定 质量标准 

分 类 号：R917[医药卫生—药物分析学]