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目的建立准确、灵敏的超声辅助固相微萃取-超快速液相色谱串联质谱(SPME-UFLC-MS/MS)测定尿液中五氯酚(PCP)的方法。方法采用聚离子液体膜(PIL)进行固相微萃取,XR-ODS II色谱柱(100 mm×2.0 mm,2.5μm)为分离柱,以甲醇-乙腈-5 mmol/L乙酸铵水溶液(15∶50∶35,V/V/V)为流动相进行分离,采用电喷雾电离负离子多反应监测模式(MRM)测定。结果尿液中PCP在1.0 ng/L~200.0 ng/L线性相关系数为0.999 1,加标回收率为89.5%~94.9%,日内相对标准偏差(RSDs)为1.3%~4.1%,日间RSDs为2.9%~6.8%,最低定量检出限为1.0 ng/L,与固相萃取方法比较差异无统计学意义。结论建立的方法简便、干扰少、特异性强,可用于尿液中痕量PCP的测定。
Objective To establish an accurate and sensitive method for the determination of pentachlorophenol (PCP) in urine by ultrasonography-assisted solid-phase microextraction-ultra-fast liquid chromatography tandem mass spectrometry (SPME-UFLC-MS / MS). Methods Solid phase microextraction was performed on poly (ionic liquid) membrane (PIL). The separation was performed on a XR-ODS II column (100 mm × 2.0 mm, 2.5 μm) 50:35, V / V / V) as the mobile phase, using electrospray ionization negative ion multiple reaction monitoring mode (MRM). Results The linear correlation coefficient (PCP) of 1.0 ng / L to 200.0 ng / L in urine was 0.999 1, the spiked recoveries were 89.5% -94.9% and the relative standard deviations (RSDs) were 1.3% -4.1% Was 2.9% ~ 6.8%, the lowest detection limit was 1.0 ng / L, which was not significantly different from that of solid-phase extraction. Conclusion The method is simple, less interference and specific, and can be used for the determination of trace PCP in urine.