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采用高通量固相萃取和超高效液相色谱/串联质谱法测定食品和饮用水中的全氟化学品。

Determination of perfluorinated chemicals in food and drinking water using high-flow solid-phase extraction and ultra-high performance liquid chromatography/tandem mass spectrometry.

机构信息

Institute of Environmental Health, College of Public Health, National Taiwan University, Taipei 10055, Taiwan.

出版信息

Anal Bioanal Chem. 2012 Jan;402(3):1315-25. doi: 10.1007/s00216-011-5519-9. Epub 2011 Nov 10.

DOI:10.1007/s00216-011-5519-9
PMID:22071607
Abstract

For this study, we developed methods of determining ten perfluorinated chemicals in drinking water, milk, fish, beef, and pig liver using high-flow automated solid-phase extraction (SPE) and ultra-high performance liquid chromatography/tandem mass spectrometry. The analytes were separated on a core-shell Kinetex C18 column. The mobile phase was composed of methanol and 10-mM N-methylmorpholine. Milk was digested with 0.5 N potassium hydroxide in Milli-Q water, and was extracted with an Atlantic HLB disk to perform automated SPE at a flow rate ranged from 70 to 86 mL/min. Drinking water was directly extracted by the SPE. Solid food samples were digested in alkaline methanol and their supernatants were diluted and also processed by SPE. The disks were washed with 40% methanol/60% water and then eluted with 0.1% ammonium hydroxide in methanol. Suppression of signal intensity of most analytes by matrixes was lower than 50%; it was generally lower in fish and drinking water but higher in liver. Most quantitative biases and relative standard deviations were lower than 15%. The limits of detection for most analytes were sub-nanograms per liter for drinking water and sub-nanograms per gram for solid food samples. This method greatly shortened the time and labor needed for digestion, SPE, and liquid chromatography. This method has been applied to analyze 14 types of food samples. Perfluorooctanoic acid was found to be the highest among the analytes (median at 3.2-64 ng/g wet weight), followed by perfluorodecanoic acid (0.7-25 ng/g) and perfluorododecanoic acid (0.6-15 ng/g).

摘要

本研究采用高通量自动固相萃取(SPE)和超高效液相色谱/串联质谱法,开发了测定饮用水、牛奶、鱼类、牛肉和猪肝中十种全氟化合物的方法。分析物在核壳 Kinetex C18 柱上分离。流动相由甲醇和 10mM N-甲基吗啉组成。牛奶用 0.5N 氢氧化钾在 Milli-Q 水中消化,用 Atlantic HLB 盘提取,以 70-86mL/min 的流速进行自动 SPE。饮用水直接用 SPE 提取。固体食品样品在碱性甲醇中消化,上清液稀释后也用 SPE 处理。将圆盘用 40%甲醇/60%水洗涤,然后用 0.1%氨甲醇洗脱。基质对大多数分析物信号强度的抑制低于 50%;在鱼类和饮用水中通常较低,但在肝脏中较高。大多数定量偏差和相对标准偏差低于 15%。大多数分析物的检测限为饮用水纳克/升以下,固体食品样品纳克/克以下。该方法大大缩短了消化、SPE 和液相色谱所需的时间和劳动量。该方法已应用于分析 14 种食品样品。全氟辛酸是所有分析物中含量最高的(湿重中位数为 3.2-64ng/g),其次是全氟癸酸(0.7-25ng/g)和全氟十二酸(0.6-15ng/g)。

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