QuEChERS前处理技术联合液相色谱-四极杆飞行时间质谱法检测保健食品中24种违禁降血糖、降血压和降血脂药物

建立QuEChERS前处理技术联合液相色谱-四极杆飞行时间高分辨质谱(LC-Q-TOF-MS)测定保健食品中24种违禁降血糖、降血压和降血脂药物成分的分析方法。采用响应曲面设计实验优化了前处理萃取条件:乙腈与水体积比、硫酸镁与氯化钠用量和吸附剂C18用量。依据目标物的一级母离子的精确质量数、同位素丰度比、二级碎片离子的精确质量数和色谱保留时间等信息定性、定量地分析降血糖、降血压和降血脂违禁药物。结果显示,QuEChERS前处理技术与LC-Q-TOF-MS分析方法检测保健食品中违禁降血糖、降血压和降血脂药物的选择性好,检出限和定量限低,灵敏度高,线性关系良好(r²>0.997)。将该方法用于15个保健食品样品的检测,发现5个样品含有违禁药物。

Determination of 24 antihyperglycemic,antihypertensive and antihyperlipidemic drugs illegally added in health food samples by liquid chromatography-quadrupole- time of flight mass spectrometry

A liquid chromatography-quadrupole-time of flight mass spectrometry (LC-Q-TOF-MS) coupled with QuEChERS pretreatment analytical method was established for the identification and quantification of 24 antihyperglycemic, antihypertensive and antihyperlipidemic drugs illegally added in health foods. The extraction conditions, including the volume ratio of ACN and H₂O, the amount of MgSO₄ & NaCl used, and the amount of C18 used, were optimized by response surface methodology. The quantitative analysis was based on the accurate masses of the first level of parent molecular ions and isotopic patterns, and accurate masses of the second level of fragment ions and a priori known retention times. The established QuEChERS pretreatment method combined with LC-Q-TOF-MS was effective for the simultaneous characterization and quantification of antihyperglycemic, antihypertensive and antihyperlipidemic drugs with high selectivity, a high linearity (r²>0.997) in wide range, low LODs and LOQs, and high precision. The method was successfully applied to determinate the drugs illegally added in the fifteen health food samples, the five of which were positive samples.