液质联用法测定保健食品中非法添加57种化学药的研究

Rapid Determination of 57 Chemicals Illegally Added to Health Foods by UPLC-MS/MS

目的:建立一种同时完成抗风湿类、止咳平喘类保健食品中非法添加糖皮质激素和非甾体抗炎药(NSAIDs)等共57种化学药物的快速准确筛查和定性分析的方法。方法:样品采用乙腈超声提取。采用UPLC-MS/MS法,以Atlantis?dC18(150 mm×2.1 mm,3μm)为色谱柱,以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱;流速为0.3 ml·min-1,柱温为40℃,进样体积为5μl。选择ESI离子源,正离子扫描,负离子扫描;多反应监测(MRM)模式,测定57种临床常用的化学药物,通过比较MRM通道中样品峰与对照品峰的分子离子峰,二级碎片离子峰等信息确定添加的化学药。结果:在上述色谱及质谱条件下,57种化学药的质谱检测的线性范围宽,相关性好(r>0.9950);方法回收率范围在80.0%~120.0%(n=9);检测限0.0083~2.5857μg·g^-1,定量限0.0285~8.6191μg·g^-1。对160批样品进行了检测,一次检测可同时对样品中添加的57种化学成分进行筛查和定性分析,有1批次样品中检出双氯芬酸钠。结论:研究结果表明,本法专属性强,灵敏度高,可作为保健食品中非法添加57种糖皮质激素和非甾体抗炎药的快速筛查和准确定性。

Objective:To establish a rapid and accurate method for the simultaneous determination of 57 glucocorticoids and NSAIDs illegally added to health foods in a single analysis.Methods:A UPLC-MS/MS method was adopted.The samples were extracted with acetonitrile by ultrasonic processing and separated on an Atlantis■dC18(150 mm×2.1 mm,3μm)column with 0.1%formic acid water solution(A)and acetonitrile(B)as the mobile phase with gradient elution at a flow rate of 0.3 ml·min-1,and the column temperature was 40℃,the injection volume was 5μl.A positive-ion source,a negative-ion source and an MRM mode were used to separate and determine the chemicals.The obtained molecular ions,fragment ions and MRM channels were used to identify the 57 kinds of drugs by the comparison with the reference substances.Results:Totally 57 linear calibration curves were obtained with r>0.9950.The recoveries ranged from 80.0%to 120.0%(n=9).The qualitative and quantitative limits were within the range of 0.0083μg·g^-1-2.5857μg·g^-1 and 0.0285μg·g-1-8.6191μg·g^-1,respectively.The established method could complete the screening and confirmation of the 57 kinds of drugs simultaneously.Totally 160 batches of samples were tested by the method.Diclofenac sodium was detected out in one sample.Conclusion:The established method is specific and sensitive,which can be successfully used for the screening and confirmation of 57 glucocorticoids and NSAIDs illegally added to health foods.