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目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)法快速、准确地检测保健贴膏中违禁添加解热镇痛类、糖皮质激素类及抗过敏类化学药物。方法:采用Waters Acquity UPLC BEH C18(1.7μm,2.1mm×100mm)色谱柱,以0.1%甲酸的甲醇溶液为流动相A,以0.1%甲酸的水溶液为流动相B,梯度洗脱。通过分子离子峰,二级碎片、色谱保留时间等信息,对保健贴膏中的双氯芬酸钠等9种化学药物进行质谱鉴定。结果:12批保健止痛贴膏,3批被检测出同时添加了马来酸氯苯那敏和吲哚美辛,4批被检测出添加了双氯芬酸钠,2批被检测出添加了马来酸氯苯那敏,3批未检出。结论:本方法专属性强、灵敏度高,结果准确可靠,可作为贴膏剂中鉴别非法添加化学药物的有效方法。
OBJECTIVE: To establish rapid and accurate UPLC-MS / MS for the detection of antipyretic analgesics, glucocorticoids and anti-allergy chemicals in health patch. Methods: Waters Acquity UPLC BEH C18 (1.7μm, 2.1mm × 100mm) column was used. The mobile phase consisted of 0.1% formic acid in methanol and 0.1% formic acid as mobile phase. Nine chemical drugs, diclofenac sodium and so on, were identified by mass spectrometry through molecular ion peak, secondary fragment and chromatographic retention time. Results: Twelve batches of pain relief plaster were applied in three batches, while chlorpheniramine maleate and indomethacin were also added in the three batches. Diclofenac sodium was added in four batches and two batches were detected with addition of maleic acid chloride Benzene Min, 3 batches not detected. Conclusion: The method is highly specific, sensitive and accurate and reliable. It can be used as an effective method to identify the illegal addition of chemical drugs in the patch.