Lin Qin, Fu Fengfu, Chen Guonan, Zheng Xiaoyan, Dai Ming
Se Pu. 2014 Jul;32(7):723-9. doi: 10.3724/sp.j.1123.2014.03023.
A method for the determination of six perfluorinated organic compounds (PFCs) in feed has been developed. It is based on polyamide solid-phase extraction (SPE) together with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted by acidified acetonitrile. The extraction solution was enriched by a polyamide SPE cartridge under acidic condition, and cleaned-up using methanol, eluted by 5% (v/v) ammonia/methanol solvent and determined by UPLC-MS/MS. The UPLC separation was carried out on an Acquity BEH C18 column (100 mm x 2.1 mm, 1.7 microm). The mobile phases were 5 mmol/L ammonium acetate and acetonitrile with a gradient elution. Under the optimal conditions, the PFCs were analyzed under multiple reaction monitoring (MRM) mode with negative electrospray ionization. The isotope internal standard method was used to determine the six PFCs, and improve the quantitative accuracy. All of the target compounds exhibited good linearity (r > 0.995) over a concentration range of 0.5-25 microg/L. The detection limits of the six PFCs were all smaller than 0.1 microg/kg. The mean recoveries of the six PFCs were in the range of 94.2% to 108.9% with the relative standard deviations (RSDs) of 1.8% - 8.6% (n = 6). The method for the determination of PFCs in feed is low-cost, favorable effect and suitable for the detection of complex matrix samples.
建立了一种测定饲料中六种全氟有机化合物（PFCs）的方法。该方法基于聚酰胺固相萃取（SPE）结合超高效液相色谱-串联质谱（UPLC-MS/MS）。样品用酸化乙腈萃取。萃取液在酸性条件下通过聚酰胺SPE柱富集，用甲醇净化，用5%（v/v）氨/甲醇溶剂洗脱，然后用UPLC-MS/MS测定。UPLC分离在Acquity BEH C18柱（100 mm×2.1 mm，1.7μm）上进行。流动相为5 mmol/L乙酸铵和乙腈，采用梯度洗脱。在最佳条件下，PFCs在负离子电喷雾电离的多反应监测（MRM）模式下进行分析。采用同位素内标法测定六种PFCs，提高了定量准确性。所有目标化合物在0.5-25μg/L的浓度范围内均表现出良好的线性（r>0.995）。六种PFCs的检出限均小于0.1μg/kg。六种PFCs的平均回收率在94.2%至108.9%之间，相对标准偏差（RSDs）为1.8%-8.6%（n = 6）。该饲料中PFCs的测定方法成本低、效果好，适用于复杂基质样品的检测。
