UPLC-MS/MS法检测洁白制剂中沉香的使用情况  

Determination of the use of agarwood in Jiebai preparations by UPLC-MS/MS

作　　者：武嘉庚 杨凤梅 张炜 范莹莹 WU Jia-geng;YANG Feng-mei;ZHANG Wei;FAN Ying-ying(Qinghai Key Laboratory of Modernization of Traditional Chinese and Tibetan Medicine,Qinghai Provincial Drug inspection and Testing Institute,Xining 810016,China)

机构地区：[1]青海省药品检验检测院/青海省中藏药现代化研究重点实验室

出　　处：《实用药物与临床》2019年第12期1303-1306,共4页Practical Pharmacy and Clinical Remedies

基　　金：藏成药“洁白制剂”质量控制及安全性评价研究(2017-ZJ-772);青海省科技厅科技基础条件平台项目(2017-ZJ-Y40)

摘　　要：目的建立超高效液相色谱-串联电喷雾三重四级杆质谱(UPLC-MS/MS)法,通过对沉香四醇含量测定,对洁白胶囊(丸)中沉香的使用情况进行检测。方法该药物乙醇提取物的分析采用电喷雾离子源(ESI)进行电离,多离子反应监测(MRM)模式进行信号采集,采用外标法进行定量;以乙腈-0.1%甲酸溶液(75∶25)为流动相;等度洗脱;体积流量:0.3 ml/min;柱温:40℃,测定洁白胶囊(丸)中沉香四醇含量。结果50批洁白胶囊(丸)中有29批沉香四醇含量过低,提示企业可能投劣质沉香,3批洁白丸未检出沉香四醇,提示可能未投沉香或以山沉香代替投料。结论该方法选择性强,灵敏度高,可用于测定洁白胶囊(丸)中沉香四醇含量,检测洁白胶囊(丸)中沉香使用情况,确保沉香药材的质量可控。Objective To establish an UPLC-MS/MS method for the determination of agarotetrol content to detect the use of agarwood in Jiebai Capsule(pill).Methods The analysis of ethanol extract of this drug was carried out on an ESI for ionization.MRM was used to acquire the signal,and quantification was performed by external standard method.The mobile phase consisted of acetonitrile-0.1%formic acid in water(75∶25)with equal elution.The flow rate was 0.3 ml/min,and the column temperature was 40℃.The content of agarotetrol in Jiebai Capsule(pill)was detected.Results There were 50 batches of Jiebai Capsules(pill),and 29 batches of them had low contents of agarotetrol,which showed that companies might add low-quality agarwood.Agarotetrol could not be detected in 3 batches of Jiebai Capsule,suggesting that the agarwood might not be used or be replaced by Ramulus syringae.Conclusion This method is specific,sensitive and suitable for the content determination of agarotetrol;it can investigate the use of agarwood in Jiebai Capsule(pill),so that the quality can be controlled.

关 键 词：洁白胶囊(丸) 沉香 沉香四醇 UPLC-MS/MS 

分 类 号：R28[医药卫生—中药学]