分散固相萃取-高效液相色谱-串联质谱法测定白酒中全氟化合物方法研究

食品科学 ›› 2013, Vol. 34 ›› Issue (22): 143-149.

分散固相萃取-高效液相色谱-串联质谱法测定白酒中全氟化合物方法研究

冯沙¹,蓝芳²,吴晓萍³,沈金灿²,岳振峰²,熊贝贝²

1. 湛江海洋大学
2. 深圳出入境检验检疫局
3. 广东海洋大学食品科技学院

收稿日期:2013-05-26 修回日期:2013-10-15 出版日期:2013-11-25 发布日期:2013-12-05
通讯作者: 沈金灿 E-mail:jincansh@263.net
基金资助:
化学消毒食品中氨基脲的产生机理及控制措施研究

Determination of 15 perfluorinated compounds in Chinese spirit by dispersive solidphase extraction and HPLC-MS/MS detection

Received:2013-05-26 Revised:2013-10-15 Online:2013-11-25 Published:2013-12-05

摘要/Abstract

摘要：

建立了白酒中15种全氟化合物的分散固相萃取-高效液相色谱-串联质谱快速分析方法。1.0 mL白酒样品以50 mg PSA吸附剂进行富集净化，用50 mmol/L三乙胺-甲醇液洗脱后，采用HPLC-ESI-MS/MS电喷雾负离子模式电离，多反应监测模式对样品进行检测，内标法进行定量分析。15种全氟化合物在0.1-20μg/L浓度范围内呈良好的线性关系，方法的检出限为0.03-0.15μg/L，定量限为0.10-0.45 μg/L。在0.5、1.0、2.0和5.0μg/L四种添加水平下，15种全氟化合物的加标回收率为83.8%-119%。

Abstract:

A rapid dispersive solidphase extraction and HPLC-MS/MS detection method was developed for the determination of 15 perfluorinated compounds in Chinese spirit. 1.0 mL sample was extracted by 50 mg PSA dispersive solidphase extraction and eluted with 50 mmol/L triethylamine-methanol solution. Then the extract was further detected by HPLC-MS/MS. Analysis was performed by electrospray ionization in negative mode with multiple reaction monitoring(MRM) using internal standard method for quantitative determination. Good linearities were established for the 15 PFCs in the range from 0.1μg/L to 20.0μg/L. The limits of detection were between 0.03 and 0.15μg/L, while the limits of quantitation were ranged from 0.09 to 0.45μg/L. The average recoveries of 15 PFCs were between 83.8% and 119% in spiking levels of 0.5, 1.0 , 2.0and 5.0μg/L.

中图分类号:

O656.3

冯沙蓝芳吴晓萍沈金灿岳振峰熊贝贝. 分散固相萃取-高效液相色谱-串联质谱法测定白酒中全氟化合物方法研究[J]. 食品科学, 2013, 34(22): 143-149.

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