简单稀释UHPLC-MS/MS法测定抗风湿制剂中12种非法添加药物

Determination of 12 Antirheumatic Drugs in Illicit Preparations by Simple Dilution-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

目的:建立制剂中非法添加抗风湿药物的超液相色谱-串联质谱(UHPLC-MS/MS)检测方法。方法:样品经甲醇稀释,以Poroshell 120为分析色谱柱,以甲醇和甲酸-乙酸铵水溶液为流动相,梯度淋洗分离,经电喷雾离子源电离后质谱检测。结果:阿司匹林,布洛芬,萘普生,对乙酰氨基酚,氨基比林,甲氧苄啶,双氯芬酸钠,吡罗昔康,吲哚美辛,氢化可的松,地塞米松,醋酸泼尼松12种物质线性关系良好,回收率、RSD均能满足检验需求。结论:简单稀释进样,避免了设备污染,基质效应,为非靶向筛查非法添加药物的检测技术提供参考依据。

Objective:To develop aUltra-liquid chromatography-tandem mass spectrometry method(UHPLC-MS/MS)for the detection of antirheumatic drugs in illegal preparations.Methods:The samples were diluted by methanol,and the drugs in the sample solution were separated by gradient elution using Poroshell 120 as the analytical column with methanol and aqueous formic acid-ammonium acetate as the mobile phases,and detected by mass spectrometry after ionization with an electrospray ionization source.Results:The linearity of the 12 substances was good for aspirin,ibuprofen,naproxen,acetaminophen,aminopyrine,meperidine,diclofenac sodium,piroxicam,indomethacin,hydrocortisone,dexamethasone and prednisone acetate,and the recoveries and RSDs could meet the test requirements.Conclusion:Simple dilution injection can avoid equipment contamination and matrix effects,and lay a solid foundation for non-targeted screening of illegally added drugs.