超高效液相色谱-串联质谱法检测茶制品中非法添加13种抗风湿类药物

Determination of 13 kinds of anti-rheumatic drugs illegally added illegally in tea products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  茶制品  抗风湿类药物  超高效液相色谱-串联质谱法

英文关键词:tea products  anti-rheumatic drugs  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法检测茶制品中非法添加13种抗风湿类药物(氨基比林、对乙酰氨基酚、甲氧苄啶、氢化可的松、吡罗昔康、醋酸泼尼松、地塞米松、双氯芬酸钠、吲哚美辛、保泰松、罗通定、安替比林、非那西丁)的分析方法。方法 样品甲醇超声提取后, 以0.1%的甲酸溶液-乙腈为流动相梯度洗脱, 经Inertsil ODS-3(2.1 mm×75 mm, 2 μm)色谱柱分离, 目标化合物在ESI源正离子模式下电离, 采用多反应监测模式进行定性、定量分析。结果 13种抗风湿的方法检出限(S/N=3)为0.3~1.6 μg/kg, 定量限(S/N=10)为1.4~6.5 μg/kg。在低、中、高3个加标水平下的平均回收率为80.20%~110.31%。对25批次市售抗风湿类茶制品进行检测, 均未发现上述13种抗风湿类药物。结论 该方法灵敏高、专属性强, 适用于茶制品中抗风湿类非法添加的定量及确证分析。

英文摘要:

      Objective To establish a method for rapid determination of 13 kinds of anti-rheumatic drugs (aminophenazone, 4-acetamidophenol, trimethoprim, hydrocortisone, piroxicam, prednisone 21-acetate, dexamethasone, phenacetin, indometacin, phenylbutazone, rotundine, phenazone, diclofenac sodium) added in tea products by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with methanol by ultrasonication. After chromatographic separation on an Inertsil ODS-3 (2.1 mm×75 mm, 2 μm) column with 0.1% formic acid solution-acetonitrile as mobile phase, the target compounds were qualitatively and quantitatively determined under the multiple reaction monitoring (MRM) mode in positive ionization mode. Results The limits of detection (LOD) for 13 anti-rheumatic were in the range of 0.3?1.6 μg/kg and the limits of quantification (LOQ) were in the range of 1.4?6.5 μg/kg. The average recoveries at three spiked levels ranged from 80.20% to 110.31%. None of the 13 anti-rheumatic drugs were found in 25 batches of commercially available anti-rheumatic tea products. Conclusion This method is sensitive, sufficiently selective and is suitable for the determination and confirmation of 13 anti-rheumatic in tea products.