分散液液微萃取/HPLC-MS/MS测定保健茶中非甾体抗炎药

Dispersive Liquid-Liquid Microextraction Coupled with HPLC-MS/MS in the Analysis of Anti-inflammatory Drugs in Healthy Tea

建立同时检验保健茶中9种非甾体抗炎药的分散液液微萃取/超高效液相色谱-线性离子阱串联质谱(UP-LC-MS/MS)的方法。样品采用乙腈提取,提取液用分散液液微萃取(DLLME)处理,然后用C_(18)超高效液相色谱柱(2.1 mm×100 mm,1.6μm)分离,以0.05%(V/V)甲酸的2 mmol/L乙酸铵溶液和乙腈为流动相,流速0.4 m L/min,柱温35℃。采用电喷雾正离子多反应监测(MRM)模式进行检测,外标法定量。9种非甾体抗炎药的浓度和峰面积在各自浓度范围内呈现良好线性关系,相关系数(r)均大于0.998;检出限为0.5~5μg/kg,定量限为1.5~15μg/kg;在0.02,0.05和0.2 mg/kg个添加水平下,9种待测化合物的平均回收率为85.7%~105.7%,相对标准偏差(S;)为1.7%~8.9%(n=6)。该方法分析速度快,准确可靠,适用于保健茶中9种非甾体抗炎药检测。

A method for determination of 9 nonsteroidal anti-inflammatory drugs in healthy tea based on ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with liquid-liquid micro-extraction(DLLME)procedure was developed.The samples were extracted with acetonitrile,and then purified concentrated by DLLME,the 9 antiinflammatory drugs in extracted solution were separated on the HPLC C_(18)chromatographic column(2.1 mm×100 mm,1.6μm)with 2 mmol/L ammonium acetate formate solution containing 0.05%(V/V)formic acid and acetonitrile as mobile phase,at a flow rate of 0.4 m L/min,and the column temperature was 35℃.The electrospray positive ion multiple reaction monitoring(MRM)mode was used for detection and quantification by external standard method.There was a good linear relationship between the concentration and peak area of the nine compounds,and the correlation coefficients(r)were all greater than 0.998.The limits of detection were 0.5-5μg/kg,and the limits of quantification were 1.5-15μg/kg.The average recoveries of the nine compounds were in the range of 85.7%-105.7%with relative standard deviations(S;)of 1.7%-8.9%(n=6)at 0.02,0.05and 0.2 mg/kg supplemental levels.This method is fast,accurate and reliable,and can be used for the determination of 9 antiinflammatory compounds in healthy tea.