液相色谱-串联质谱法测定水产品中壬基酚和辛基酚

Determination of Nonylphenol and Octylphenol in Aquatic Productby Liquid Chromatography Tandem Mass Spectrometry

建立水产品中壬基酚和辛基酚的液相色谱-串联质谱（HPLC-MS/MS）检测方法。采用乙腈超声提取,经PSA固相萃取柱净化后。采用Waters Sun Fire C18色谱柱,以0.1%氨水甲醇-0.1%氨水溶液为流动相,在HPLC-MS/MS多反应监测模式下进行定性与定量分析。壬基酚和辛基酚的方法检出限均为1μg/kg,在10~100μg/kg的3个添加水平范围内,平均回收率为60%~120%,相对标准偏差均小于20%。本方法准确、快速和灵敏度高,可用于水产品检验。

A comprehensive analytical method based on liquid chromatography tandem mass spectrometry （HPLC-MS/ MS） has been developed for determination of nonylphenol and octylphenol in aquatic product. Analytes were extracted by acetoui- trile and purified by PSA solid phase extraction cartridge. Qualitative and quantitative analyses were carried out for analytes under multiple reaction monitoring （MRM） mode after chromatographic separation oll Waters SunFire C18 （50 mm×2.hnm, 3.5μm） column with methanol-0.1% NH4OH. Limits of detection （LODs） for nonylphenol and octylphenol were 1 μg/kg. Mean recover- ies at spiked level of 10~100μg/kg were 60%~1 20%, with relative standard deviation less than 20%. This method is accurate, simple, rapid and adapts to inspection of nonylphenol and octylphenol in aquatic product.