含乳食品中17种塑化剂的检测

Determination of 17 plasticizers in dairy food

目的采用固相萃取-超高效液相色谱-串联质谱技术(UPLC-MS/MS),建立含乳食品中17种塑化剂的检测方法。方法样品采用乙腈提取,经OASIS Prime HLB固相萃取柱净化。以BEH Phenyl(2.1 mm×100 mm×1.7μm)色谱柱进行色谱分离,以电喷雾电离(ESI)串联质谱多反应检测模式(MRM)进行监测,同位素内标标准曲线法定量。结果 17种塑化剂化合物在0.5~500μg/L浓度范围内呈良好的线性关系,R^2>0.9990,检出限为1~14μg/kg,加标回收率(n=6)为89.8%~119.0%,相对标准偏差(RSD)为3.62%~12.60%,具有良好的重现性。结论UPLC-MS/MS法简单、准确、灵敏度高,特别是样品前处理快捷简便,适用于含乳食品中17种塑化剂的检测。

Objective A method was established for determination of 17 kinds of plasticizers in infant formula by solid-phase extraction coupled with UPLC-MS / MS.Methods The plasticizers were extracted from the infant formula with acetonitrile,and purified by solid phase extraction column named OASIS Prime HLB. The analytes were then separated by the chromatographic column（ BEH Phenyl,2. 1 mm × 100 mm × 1. 7μm）. The ion fragment information analytes were obtained using ultra high performance liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode and the isotope internal standards were used to quantify by calibration curves. Results The method showed a good linearity（ R-2 0. 9990） in the range of 0. 5- 500 μg / L for17 plasticizers analytes with average recovery rates of 89. 8%- 119. 0%（ n = 6） and the relative standard deviation（ RSD） within 3. 62%- 12. 60%. The limits of quantification（ LOQ） were between 1 μg /kg and 14 μg /kg. Conclusion The method is simple,sensitive and accurate,and the sample pretreatment is very convenient especially,is suitable for the determination of 17 plasticizers in infant formula and dairy products.