高效液相色谱-串联质谱法检测保健食品中25种非甾体类抗炎药

Determination of 25 kinds of non-steroidal anti-inflammatory drugs in dietary supplements by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  非甾体类抗炎药  保健食品  高效液相色谱-串联质谱法

英文关键词:non-steroidal anti-inflammatory drugs  dietary supplements  high performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)分析保健食品中25种非法添加非甾体类抗炎药(non-steroidal anti-inflammatory drugs, NSAIDs)的分析方法。方法 保健食品固体试样经甲醇超声提取, 液体试样经水-甲醇萃取来提取, 经液相色谱柱分离后, 在多反应监测(multiple reaction monitoring, MRM)模式下测进行25种NSAIDs含量的测定, 外标法定量。结果 25种非甾体抗炎药在1~500 ng/mL范围内呈现良好线性关系, 相关系数均大于0.99, 检出限为1.5~2.0 μg/kg, 定量限为5.0~6.0 μg/kg, 6.0、12.0和60.0 μg/kg 3个水平平均加标回收率为80.0%~108.2%, 相对标准偏差为6.4%~9.9% (n=6)。结论 该方法针对保健食品基质, 对固体和液体样品分别采取超声萃取和液液直接萃取的提取方式, 操作简便、节约成本、专属性强且灵敏度、回收率高, 满足保健食品中NSAIDs的检测。

英文摘要:

      Objective To establish a method for the determination of 25 kinds of non-steroidal anti-inflammatory drugs (NSAIDs) illegally added to dietary supplements by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The analytes were extracted from the solid samples by ultrasound-assisted extraction and extracted from the liquid samples by liquid-liquid extraction both using methanol as extractant. After separated by liquid chromatography column, the content of 25 kinds of NSAIDs was finally determined under multiple reaction monitoring (MRM) mode by external standard method. Results The 25 kinds of NSAIDs showed a good linear relationship in the range of 1?500 ng/mL, with the correlation coefficient all greater than 0.99, the limits of detection and limits of quantitation were 1.5?2.0 μg/kg and 5.0?6.0 μg/kg, respectively. The average recoveries ranged between 80.0% and 108.2% at spiked levels of 6.0, 12.0 and 60.0 μg/kg, respectively, with relative standard deviations varying from 6.4% to 9.9% (n=6). Conclusion This method has proved to be applicable for solid and liquid samples by ultrasound-assisted and liquid-liquid extraction, respectively. This method offers high overall recoveries with substantial convenience, low cost, strong specificity and excellent sensitivity, fulfilling all requirements of the determination of NSAIDs in dietary supplements.