UPLC-MS/MS检测压片糖果类食品中非法添加的13种ARB类和利尿剂降压成分

Determination of 13 Kinds of Illegally Added ARB and Diuretic Antihypertensive Drugs in Compressed Candy Products by UPLC-MS/MS

目的建立压片糖果类食品中非法添加的13种血管紧张素II受体拮抗剂(ARB)和利尿剂降压成分的UPLC-MS/MS分析方法。方法样品用甲醇经超声提取,经SB-C_(18)色谱柱(100 mm×2.1 mm,2.7μm)分离,以5 mmol/L甲酸铵水溶液和乙腈作为流动相,进行梯度洗脱,在正离子和负离子扫描模式下,采用MRM模式检测。结果阿齐沙坦、替米沙坦、氯沙坦、美托拉宗等13种成分在0.5~10μg/L质量浓度范围内均线性良好。相关系数(r)为0.9951~0.9995。在0.125,0.25,1.25 mg/kg水平下,压片糖果基质中的加标回收率为85.0%~115.0%。13种成分检出限为50μg/kg,定量限为125μg/kg。结论本方法简单、快速、可靠、灵敏度高,可用于压片糖果中非法添加ARB类和利尿剂降压成分的定性及定量检测。

Objective To establish an analytical method for the determination of 13 kinds of illegally added ARB and diuretic drugs in compressed candy products by UPLC-MS/MS.Methods The samples were ultrasonically extracted by methanol,separated on a SB-C_(18)column(100 mm×2.1 mm,2.7μm),using 5 mmol/L ammonium formate and acetonitrile as the mobile phase for gradient elution.In the positive and negative ion scanning mode,MRM was used for detection.Results 13 kinds of ARB and diuretic drugs including azilsartan,telmisartan,losartan,metolazone,and so on,showed good linearity in the mass concentration range of 0.5-10μg/L.The correlation coefficients were 0.9951-0.9995.The recoveries at spiked levels of 0.125,0.25,1.25 mg/kg ranged from 85.0%to 115.0%.The limit of detection of 13 kinds of ARB and diuretic drugs was 50μg/kg and the limit of quantification was 125μg/kg.Conclusion The method developed in this study is simple,fast,convenient and sensitive,and can be used for the qualitative and quantitative analysis of ARB or diuretic drugs in compressed candy products.