不同厂家八宝惊风散中人工牛黄胆汁酸类活性成分的含量测定及差异分析  

Determination and difference analysis of bile acid active constituents of artificial bezoar in Babao jingfeng powder from different manufacturers

作　　者：钟琪[1] 陈伟康 周国平 刘艳梅 刘德鸿 李晶[3] ZHONG Qi;CHEN Weikang;ZHOU Guoping;LIU Yanmei;LIU Dehong;LI Jing(Dept.of Pharmacy,ThePeople’s Hospital of Ganzhou,Jiangxi Ganzhou 341000,China;Jiangxi Institute for Drug Control/NMPAKey Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine/Jiangxi Provincial EngineeringResearch Center of Drug and Medical Device Quality,Nanchang 330029,China;Jiangxi Provincial Instituteof Traditional Chinese Medicine,Nanchang 330029,China)

机构地区：[1]赣州市人民医院药剂科,江西赣州341000 [2]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 [3]江西省中医药研究院,南昌330029

出　　处：《中国药房》2023年第20期2502-2506,共5页China Pharmacy

基　　金：江西省中医药中青年骨干人才(第一批)培养计划项目(No.赣中医药科教字〔2020〕2号)。

摘　　要：目的建立同时测定八宝惊风散中人工牛黄有效成分(胆酸、猪去氧胆酸和牛磺胆酸钠)含量的方法,比较不同厂家样品中3个成分的含量差异。方法采用超高效液相串联质谱法测定3个厂家9批八宝惊风散中胆酸、猪去氧胆酸和牛磺胆酸钠的含量,色谱柱为Phenomenex Luna®C18,流动相为乙腈-水(梯度洗脱),流速为0.5 mL/min,柱温为40℃,进样量为2μL。质谱采用负离子单四极杆模式,胆酸、猪去氧胆酸和牛磺胆酸钠的m/z分别为407.2、392.2、514.2。以3个成分的含量为指标,对9批样品进行聚类分析和主成分分析。结果胆酸、猪去氧胆酸和牛磺胆酸钠的线性范围分别为5.48~548.40、5.38~538.40、4.74~474.05 ng/mL(r≥0.9993);精密度、重复性、稳定性(24 h)的RSD均不高于3.7%(n=6),平均回收率分别为103.3%、103.3%、101.6%,RSD分别为3.3%、3.4%、4.2%(n=6)。9批样品中胆酸、猪去氧胆酸、牛磺胆酸钠的含量分别为0.702~1.711、0.599~2.049、0.664~1.752 mg/g。A厂家样品中3个成分的平均含量较高,批间差异最小;C厂家样品中3个成分的平均含量最低,批间差异较大。聚类分析基本可以区分不同厂家的样品;以主成分综合得分为指标进行聚类分析,结果与含量聚类分析结果基本一致。结论成功建立了同时测定八宝惊风散中人工牛黄3个胆汁酸类有效成分含量的方法。各厂家样品中3个成分的含量存在较大差异。OBJECTIVE To establish the method for determination of bile acid active constituents(cholic acid,hyodeoxycholic acid and sodium taurocholate)in Babao jingfeng powder,and to compare the differences of 3 constituents in Babao jingfeng powder from different manufacturers.METHODS UPLC-MS method was adopted to determine the contents of cholic acid,hyodeoxycholic acid and sodium taurocholate in 9 batches of Babao jingfeng powder from 3 manufacturers.The separation was performed on a Phenomenex Luna®C18 column with mobile phase consisted of acetonitrile-water(gradient elution)at a flow rate of 0.5 mL/min.The column temperature was 40℃and the sample size was 2μL.MS system was operated in a negative ion single quadrupole mode,and the m/z of cholic acid,hyodeoxycholic acid and sodium taurocholate were 407.2,392.2 and 514.2,respectively.With the contents of three components as the index,cluster analysis and principle component analysis were performed on 9 batches of samples.RESULTS The linear ranges of cholic acid,hyodeoxycholic acid and sodium taurocholate were 5.48-548.40,5.38-538.40,4.74-474.05 ng/mL,respectively(r≥0.9993).RSDs of precision,repeatability and stability tests(24 h)were all lower than or equal to 3.7%(n=6),and the average recoveries were 103.3%,103.3%and 101.6%with RSDs of 3.3%,3.4%,4.2%(n=6),respectively.The contents of cholic acid ranged 0.702-1.711 mg/g,those of deoxycholic acid ranged 0.599-2.049 mg/g,and those of sodium taurocholate ranged 0.664-1.752 mg/g in 9 batches of samples.The average content of 3 components in samples from manufacturer A was high,and the difference between batches was the smallest;the average content of 3 components from manufacturer C was the lowest,and the difference between batches was large.Cluster analysis could basically distinguish samples from different manufacturers;cluster analysis was conducted by using the comprehensive score of principal components as an indicator,the results of which were basically consistent with those of cluster analysis for content.CONCLU

关 键 词：八宝惊风散 胆酸 猪去氧胆酸 牛磺胆酸钠 人工牛黄 含量测定 

分 类 号：R927.2[医药卫生—药学]