摘要
目的:建立采用超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定中药材及饮片中29种合成着色剂的方法。方法:中药材以70%乙醇为提取溶剂进行超声提取,离心后取上清液以Acquity TM UPLC BEH C_(18)色谱柱(1.7μm,2.1 mm×100 mm)进行分离,以0.02 mol·L^(-1)醋酸铵溶液和甲醇为流动相进行梯度洗脱,流速为0.2 mL·min^(-1)。采用电喷雾离子源进行正离子模式监测,选择反应监测模式(SRM)用于定量分析。结果:在相应的浓度范围内,29种色素的质量浓度与峰面积呈良好的线性关系,r≥0.95;检测下限在0.1~0.26 ng之间;平均回收率范围为86.3%~116.3%,方法的相对标准偏差为0.61%~3.76%。结论:该方法分析速度快,灵敏度高,检测的色素种类较为全面,可用于中药材中非法染色的筛查。
Objective：To establish a method for simultaneous determination of 29 kinds of synthetic colorants in Chinese herbal medicine by ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）.Methods：Chinese herbal medicine was extracted with ultrasonic by 70% ethanol.Supernatant liquid was collected after centrifugation and separated on Waters Acquity TM UPLC BEH C（18） chromatographic column（1.7 μm,2.1 mm×100 mm）.0.02 mol·L^-1 ammonium acetate and methanol were used as mobile phase to elute at 0.2 mL·min^-1;Selective-reaction monitoring（SRM）scanning was employed for quatification with switching electrospragion source polarity in positive mode.Results：There was a good linear relationship between the mass concentration of 29 pigments and the peak area in the corresponding concentration range（r ≥0.95）.The detection limit was between 0.1 and 0.26 ng.The average recovery range was 86.3%-116.3%.The relative standard deviation of the method was 0.61%-3.76%.Conclusion：This analysis method has high efficiency and high sensitivity,and detection of pigment types is more comprehensive.Therefore,it can be used for the screening of illegal dyeing in Chinese herbal medicines.
作者
朱日然
韩相宁
张亚楠
朱青
ZHU Ri-ran;HAN Xiang-ning;ZHANG Ya-nan;ZHU Qing(Affiliated Hospital of Shandong University of Traditional Chinese Medicine, Jinan 250011, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第6期1029-1035,共7页
Chinese Journal of Pharmaceutical Analysis
关键词
超高效液相色谱-串联质谱(UPLC-MS/MS)
中药材
快速筛查
合成染色剂
ultra performance liquid chromatography tandem mass spectrometry （ UPLC-MS/MS ）
Chinese herbalmedicine
rapid screening
synthetic colorants
