RRLC-MS/MS法同时测定保健食品中31种降糖、降压、降血脂类非法添加化学药物  

Determination of 31 Anti-diabetic,Anti-hypertensive and Anti-hyperlipemia Compounds Illegally Added to Health Foods by RRLC-MS/MS

作　　者：王超 祝波 杨钊 Wang Chao;Zhu Bo;Yang Zhao(Qingdao Institute for Food and Drug Control,Shandong Qingdao 266071, China)

机构地区：[1]青岛市食品药品检验研究院

出　　处：《中国药师》2019年第10期1946-1950,共5页China Pharmacist

摘　　要：目的:建立同时测定保健食品中31种降糖、降压、降血脂类非法添加化学药物的快速液相色谱-串联四级杆质谱(RRLC-MS/MS)方法。方法:供试品以甲醇为提取溶剂,用甲醇-水(2∶8)稀释,经Agilent ZORBAX Eclipse Plus C18Rapid Resolution HD色谱柱(50 mm×3.0 mm,1.8μm)分离,以0.1%的甲酸溶液为流动相A,乙腈-甲醇(1∶1)为流动相B,梯度洗脱。质谱采用ESI源,正负模式同扫,动态多反应监测模式。以保留时间、定性离子对、离子比率进行定性分析,以定量离子对峰面积进行外标法定量分析。结果:31种化合物在线性范围内相关性均较好,相关系数均大于0.997 0;平均回收率为95.7%~100.5%,RSD为0.8%~2.7%;检出限在9.6~983.6 ng·g^-1之间;单次分析仅需10 min。结论:该方法专属性较好、灵敏度较高、快速、简便,适应于31种降糖、降压、降血脂类非法添加化学药物的筛查和确证。Objective: To establish a method for the determination of 31 anti-diabetic,anti-hypertensive and anti-hyperlipemia compounds illegally added to health foods by RRLC-MS/MS. Methods: The samples were extracted with methanol,diluted with methanol-water( 2∶ 8),and separated on an Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HD column( 50 mm × 3. 0 mm,1. 8μm) with 0. 1% formic acid as the mobile phase A and acetonitrile-methanol( 1∶ 1) as the mobile phase B( gradient elution). Mass spectrometry used ESI source,positive and negative mode scanning,and dynamic multi-reaction monitoring mode. The samples were identified with the retention time,qualitative ion and ion ratio,and quantified with area by ESTD method. Results: The 31 compounds showed good linear relationships within the ranges of corresponding concentrations with the correlation coefficients no less than0. 997 0. The recoveries were within the range of 95. 7%-100. 5% with the RSDs of 0. 8%-2. 7%. The detection limits were 9. 6-983. 6 ng·g-1. The 31 compounds were analyzed within 10 min. Conclusion: The established method is specific,sensitive,rapid and simple for the determination of 31 anti-diabetic,anti-hypertensive and anti-hyperlipemia compounds illegally added to health foods.

关 键 词：降糖 降压 降脂 快速液相色谱-串联四级杆质谱 动态多反应监测 

分 类 号：R917[医药卫生—药物分析学]