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目的:建立一种快速、准确检测中成药及保健食品中非法添加38种糖皮质激素的方法。方法:采用超高效液相色谱-串联质谱法(UPLC-MS-MS),Acquity BEH-C_(18)色谱柱(2.1 mm×50 mm,1.7μm),流动相0.1%乙酸乙腈溶液(A)-0.1%乙酸水溶液(B)梯度洗脱,流速0.3 m L·min~(-1),柱温25℃,电喷雾电离(ESI),正离子扫描,多反应监测(MRM)模式测定38种糖皮质激素,通过比较MRM模式下各通道样品峰与对照品峰的分子离子峰、二级碎片离子峰、色谱保留时间等信息确定添加的化学药物,并根据外标法以质谱峰面积计算添加药物的准确量。结果:在上述色谱及质谱条件下,38种糖皮质激素分离度良好,方法检测限(LOD)0.3~1.6μg·L~(-1),定量限(LOQ)1.0~5.4μg·L~(-1),加样回收率在80.9%~119.4%。结论:该方法简便、准确,灵敏度高,可用于中成药及保健品中非法添加糖皮质激素的检测。
Objective: To establish a rapid and accurate detection of proprietary Chinese medicines and health food added 38 kinds of glucocorticoid method. Methods: The mobile phase consisted of 0.1% acetic acid in acetonitrile (A), mobile phase (UPLC-MS-MS) and Acquity BEH-C 18 column (Superscript +), gradient elution with 0.1% acetic acid in water (B), flow rate of 0.3 mL · min -1, column temperature of 25 ℃, electrospray ionization (ESI), positive ion scanning and multiple reaction monitoring (MRM) Glucocorticoids were determined by comparing the molecular ion peak, secondary fragment ion peak, chromatographic retention time and other information of the sample peak and reference peak of each channel in the MRM mode to determine the added chemical drugs and calculating the peak area of the mass spectrometer according to the external standard method The exact amount of medicine. Results: Under the above chromatographic and mass spectrometric conditions, the separation of 38 glucocorticoids was good with the limits of detection (LOD) of 0.3-1.6 μg · L -1 and LOQ of 1.0-5.4 μg · L -1 -1), the sample recovery rate of 80.9% ~ 119.4%. Conclusion: The method is simple, accurate and sensitive. It can be used for the detection of illegally added glucocorticoids in proprietary Chinese medicines and health products.