Wang Xiaoyan, Shen Weijian, Wang Hong, Yu Keyao, Wu Bin, Hu Guoshen, Yang Gongjun
College of Pharmacy, Chian Pharmaceutical University, Nanjing 210009, China.
Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210009, China.
Se Pu. 2019 Jan 8;37(1):32-39. doi: 10.3724/SP.J.1123.2018.07019.
A method was developed for the simultaneous determination of 10 perfluorinated carboxylic acid compounds in water by gas chromatography-mass spectrometry coupled with negative chemical ionization (GC-NCI-MS). Perfluorinated carboxylic acid compounds were derivatized by trifluoro--methyl--(trimethylsilyl) acetamide (MSTFA) as the trimethylsilyl derivatization reagent. The water sample was purified and enriched through a weak anion exchange solid phase extraction column and analyzed via GC-NCI-MS. The sample pretreatment, derivation and instrument conditions were optimized. The results showed that the linearity of the 10 perfluorinated carboxylic acid compounds was good in the range of 0.1-10 mg/L with correlation coefficients of 0.9956-0.9993. The limits of detection (LODs) and limits of quantification (LOQs) were 0.5-1.5 μg/L and 1.5-4.5 μg/L, respectively. The spiked recoveries of the blank samples ranged from 70.2% to 112.6% with the relative standard deviations (RSDs) between 2.1% and 14.5% (=6). The method is simple, sensitive, accurate and precise, and can be used to detect the 10 perfluorinated carboxylic acid compounds in water.
建立了一种气相色谱 - 质谱联用负化学电离（GC - NCI - MS）同时测定水中10种全氟羧酸化合物的方法。以三氟甲基 - （三甲基硅基）乙酰胺（MSTFA）作为三甲基硅基衍生化试剂对全氟羧酸化合物进行衍生化。水样通过弱阴离子交换固相萃取柱进行净化和富集，然后通过GC - NCI - MS进行分析。对样品预处理、衍生化及仪器条件进行了优化。结果表明，10种全氟羧酸化合物在0.1 - 10 mg/L范围内线性良好，相关系数为0.9956 - 0.9993。检测限（LOD）和定量限（LOQ）分别为0.5 - 1.5 μg/L和1.5 - 4.5 μg/L。空白样品加标回收率在70.2%至112.6%之间，相对标准偏差（RSD）在2.1%至14.5%之间（n = 6）。该方法简便、灵敏、准确、精密，可用于检测水中的10种全氟羧酸化合物。
