同位素内标-超高效液相色谱-串联质谱测定肉类中17种全氟化合物  

Determination of 17 Perfluorinated Compounds in Meat by Isotope Internal Standard-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：林永涛[1] 谢燕湘[1] 曾小元 李兆敏[1] 黄开慧 LIN Yongtao;XIE Yanxiang;ZENG Xiaoyuan;LI Zhaomin;HUANG Kaihui(Changde Center for Disease Control and Prevention,Changde 415000,China)

机构地区：[1]常德市疾病预防控制中心,湖南常德415000

出　　处：《食品安全导刊》2022年第33期73-77,共5页China Food Safety Magazine

摘　　要：目的:建立肉类中17种全氟化合物同位素内标-超高效液相色谱-串联质谱的快速测定方法。方法:样品中加入同位素内标后用乙腈/水超声萃取,经Captiva EMR-Lipi固相萃取小柱净化,采用Kinetex C18(100 mm×2.1 mm,2.6μm)反相色谱柱进行分离,用配有电喷雾离子源的三重四极杆质谱多反应离子监测模式检测,同位素内标法定量。结果:17种全氟化合物在0.2~2.0 ng·mL^(-1)线性关系良好,相关系数不低于0.993,方法检出限在0.039~0.600μg·kg^(-1),定量限在0.13~1.80μg·kg^(-1),平均加标回收率为71.4%~105.0%,相对标准偏差为1.0%~4.5%(n=6)。结论:方法快速简便,实用性强,灵敏度好,准确性高,适用于肉类中17种全氟化合物的定性和定量检测。Objective:A method for the rapid determination of 17 perfluorinated compounds(PFCs)in meat by isotope internal standard-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Method:Samples were carrying out ultrasonic extraction with acetonitrile/water after addition of isotopically labeled internal standards.The extracts were cleaned up on a Captiva EMR-Lipi solid phase extraction column.The target compounds were separated on a Kinetex C18(100 mm×2.1 mm,2.6μm)and analyzed by a triple quadruple tandem mass spectrometer with electrospray ionization source in multiple reaction monitoring(MRM)mode and analyzed by internal standard method.Result:The standard curves were linear in the ranges of 0.2~2.0 ng·mL^(-1)for 17 PFCs with correlation coefficients greater than 0.993.The limit of detection for this method was 0.039~0.600μg·kg^(-1)and the quantitative limit was 0.13~1.80μg·kg^(-1).The average recoveries were 71.4%~105.0%and the RSD ranged from 1.0%~4.5%(n=6).Conclusion:This method is simple,rapid and practical,with high precise and accurate,and suitable for the qualitative and quantitative determination of 17 PFCs in meat.

关 键 词：超高效液相色谱-串联质谱法 同位素内标法 肉类 全氟化合物 食品安全 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]