高效液相色谱-串联质谱法测定蜂蜜中20种全氟烷基化合物

发布时间：2018-08-04 14:39

【摘要】：建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定蜂蜜中20种全氟烷基化合物(PFASs)含量的分析方法。采用改进的QuEChERS方法对样品进行前处理,用含1.5%(v/v)甲酸的乙腈溶液振荡提取,C_(18)和N-丙基乙二胺(PSA)吸附剂净化,Atlantis T3 C_(18)色谱柱(150 mm×2.1 mm,3μm)分离,以含5 mmol/L乙酸铵的甲醇溶液和5 mmol/L乙酸铵溶液为流动相进行梯度洗脱。在电喷雾离子(ESI)源负离子模式下以多反应监测(MRM)扫描,采用同位素内标法进行定量分析。结果表明,20种PFASs在16 min内即可完成分离,在0.2~10μg/L范围内线性关系良好,相关系数(r)均大于0.99;检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.04~0.10μg/kg和0.10~0.20μg/kg。在0.1、0.5、1.0和2.0μg/kg加标水平下,20种PFASs的加标回收率为72.6%~113.0%,RSD为0.4%~15.9%(n=6)。该法快速、高效、准确,适用于蜂蜜样品中20种PFASs的同时检测。
[Abstract]:A method for simultaneous determination of 20 perfluoroalkyl compounds (PFASs) in honey by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established. The modified QuEChERS method was used to pretreat the samples. The chromatographic column of Atlantis T3 _ (18) (150mm 脳 2.1 mm ~ (3 渭 m) was separated by oscillating extraction of C _ (18) and N-propylethylenediamine (PSA) from acetonitrile solution containing 1.5% (v / v) formic acid. Gradient elution was carried out with methanol solution containing 5 mmol/L ammonium acetate and 5 mmol/L ammonium acetate solution as mobile phase. The (MRM) scanning was monitored by multiple reactions under the anion mode of electrospray ion (ESI) source, and the quantitative analysis was carried out by isotopic internal standard method. The results showed that 20 species of PFASs could be separated within 16 min, the linear relationship was good in the range of 0.22 渭 g / L, the correlation coefficient (r) was greater than 0.99, the detection limits (LODX / N ~ (3) and the quantification limit (LOQ) were 0.04 ~ 0.10 渭 g/kg and 0.100.20 渭 g / kg, respectively. The recoveries of 20 kinds of PFASs were 72.6% and 113.0%, respectively, at the standard levels of 0.1 渭 g/kg and 2.0 渭 g/kg. The method is rapid, efficient and accurate. It is suitable for simultaneous determination of 20 PFASs in honey samples.
【作者单位】：山东农业大学食品科学与工程学院;中国检验检疫科学研究院;
【基金】：国家科技基础性工作专项(2013FY113100)~~
【分类号】：O657.63;S896.1

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