UPLC-MS-MS快速检测中成药及保健食品中非法添加的38种糖皮质激素

Rapid Determination of 38 Glucocorticoids Illegally Added into Chinese Patent Medicines and Dietary Supplements by UPLC-MS-MS

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 method for the determination of 38 glucocorticoids which were illegally added into the Chinese patent medicines and dietary supplements. Method：The ultra-performance liquid chromatography-tandem mass spectrum（ UPLC-MS-MS） method was adopted on a Waters Acquity BEH-C_（18）（ 2. 1 mm × 50 mm,1. 7 μm） column with 0. 1% acetic acid acetonitrile solution（ A）-0. 1% acetic acid water solution（ B） as the mobile phase for gradient elution at a flow rate of 0. 3 m L·min^-1,and the column temperature was 25 ℃. Electrospray ionization（ ESI）,positive ion scanning and a multiple reaction monitoring（ MRM） mode were used to quantitatively determine 38 glucocorticoids. The added chemical components were determined by comparing the molecular ion peaks,secondary fragment ion peaks,and retention time under MRM channels between sample peaks and reference peaks. The exact amount of added medicine was calculated according to the peak area of mass spectrometry with external standard method. Result： Under the above chromatography and mass spectrometry conditions,38 glucocorticoids were well separated. The limits of detection（ LOD） and the limits of quantitation（ LOQ） of this method were in the range of 0. 3-1. 6 μg·L^-1 and1. 0-5. 4 μg·L^-1 respectively. The recovery rates were in the range of 80. 9%-119. 4%. Conclusion： This method is simple, accurate, and highly sensitive, which can be used for the determination of illegally added glucocorticoids in Chinese patent medicines and dietary supplements.