摘要
目的:建立快速、准确超高效液相质谱联用方法,检测中成药及保健品中非法添加的36种化学药物。方法:采用Waters Acquity BEH C18 (2.1 mm×100 mm,1.7 μm)色谱柱,以0.1 %的甲酸水溶液和甲醇为流动相,梯度洗脱;选择ESI离子源、正离子扫描、多反应监测(MRM)方式检测安眠、减肥、壮阳,消炎止痛、降糖、降压和平喘类共36种临床常用的化学药物,通过比较样品峰与对照品峰的保留时间确定样品中是否添加了化学药物,并根据外标法计算添加药物的准确量。结果:在上述色谱及质谱条件下,36种药物的分离度良好,方法检测限均在0.0003~0.3750 ng·g-1之间,回收率均在79.6%~120.4%之间。结论:该方法简便准确,灵敏度高,可作为保健品及中成药非法添加化学成分的快速测定方法。
Objective: To establish a rapid,accurate UPLC-MS/MS method for the determination of 36 chemicals,which were illegally added into traditional Chinese medicines and health care products. Methods: The analytes were separated on a Waters Acquity BEH C18 Column (2.1 mm×100 mm,1.7 μm) with 0.1% fomic acid and methanol as mobile phase by gradient elution.The ultra performance liquid chromatography (UPLC)-double quadrupole mass spectrometry method with a positive-ion ESI source and a MRM mode was used to separate and quantitatively determine the 36 chemicals.The retention time and peak area obtained were used to identify and determine hypnotic,anti-obesity,aphrodisiac,analgesic-antipyretic,antidiabetic,antihypertensive and antiasthmatic drugs in traditional Chinese medicines and health care products. Results: A good resolution was obtained for the 36 kinds of chemical drugs under the UPLC and MS conditions.The determination limits were in the range of 0.0003-0.3750 ng·g-1 and the standard addition recoveries were in the range of 79.6%-120.4%. Conclasion: The method is simple,rapid,accurate and highly sensitive,which can be used for the determination of illegal traditional Chinese medicines and health care products mixed with chemical drugs.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第12期2141-2147,共7页
Chinese Journal of Pharmaceutical Analysis
基金
浙江省科技厅分析测试科技计划项目(NO.2009F70023)
关键词
中成药
保健食品
非法添加
定量测定
化学药物
UPLC—MS
MS
traditional Chinese medicines
health care products
illegal addition
quantitative determination
chemicals
UPLC - MS/MS