超高效液相色谱-串联质谱法测定血清中26种有机磷酸酯类化合物

Determination of 26 Organophosphate Esters in Serum by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

采用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了血清中26种有机磷酸酯类化合物的检测方法。血清样本经乙腈沉淀蛋白后,通过HMR固相萃取小柱净化,净化液氮吹至近干,甲醇复溶后上机检测。以5mmol/L乙酸铵水溶液和甲醇为流动相,使用C_(18)色谱柱分离目标物,质谱采用电喷雾离子源(正离子模式),以多反应监测模式检测,稳定同位素内标法定量。结果表明,26种有机磷酸酯类化合物在相应质量浓度范围内线性关系良好(r^(2)>0.997),检出限为0.024~0.146 ng/mL,定量下限为0.079~0.483 ng/mL。血清样本的加标回收率为85.7%~115%,相对标准偏差为4.5%~12%。使用该方法检测实际血清样本,检出2种有机磷酸酯类化合物。该方法操作简便、灵敏度高、精密度好,适用于大批量血清样本中有机磷酸酯类化合物的痕量检测。

A detection method for 26 organophosphate esters in serum was established using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).After precipita⁃tion of protein with acetonitrile,the serum sample was purified by HMR solid phase extraction col⁃umn,and the purified liquid nitrogen was blown to near dryness.After redissolving in methanol,it was detected on the machine.With 5 mmol/L ammonium acetate aqueous solution and methanol as mobile phase,the target substances were separated by C_(18) chromatographic column.The mass spec⁃trum was detected by electrospray ion source(positive ion mode),multi reaction monitoring mode and stable isotope internal standard method.The results showed that the 26 organophosphate esters had a good linear relationship within the corresponding mass concentration range(r^(2)>0.997),with detection limits of 0.024 ng/mL to 0.146 ng/mL and quantification limits of 0.079 ng/mL to 0.483 ng/mL.The spiked recoveries of serum sample is 85.7%to 115%,with relative standard deviations of 4.5%to 12%.This method was used to detect actual serum samples,and two types of organophos⁃phate esters were detected.This method is easy to operate,highly sensitive,and has good preci⁃sion,which is suitable for the trace detection of organophosphate esters in large quantities of serum samples.