液相色谱-串联质谱法同时测定婴幼儿配方乳粉中全氟辛酸、全氟辛烷磺酸、双酚A和壬基酚残留

建立了婴幼儿配方乳粉中全氟辛酸、全氟辛烷磺酸、双酚A和壬基酚多残留的高效液相色谱-串联四极杆质谱联用测定方法。样品用水超声溶解，乙腈沉淀蛋白质，液相色谱-串联质谱测定，基质内标法定量。以Hypersil GOLD C₁₈色谱柱（50 mm×4.6 mm，1.9 μm）分离，流动相为30 mmol/L乙酸铵水溶液和甲醇，流速0.30 mL/min。在该优化条件下，全氟辛酸、全氟辛烷磺酸、双酚A和壬基酚的定量限分别为0.5、1.0、10.0和5.0 μg/kg，方法回收率为86.1%~106.8%，相对标准偏差为2.87%~9.53%。测定了多种市售婴幼儿配方奶粉，表明该方法操作简单、测定结果准确，可用于婴幼儿配方奶粉中全氟辛酸、全氟辛烷磺酸、双酚A和壬基酚多残留的同时快速测定。

Simultaneous determination of perfluoric acid,perfluorooctane sulfonic acid,bisphenol A,nonylphenol in infant milk powder by high-performance liquid chromatography-tandem mass spectrometry

A rapid confirmative method was developed for determining the residues of perfluoric acid (PFOA), perfluorooctane sulfonic acid (PFOS), bisphenol A (BPA), and nonylphenol (NP) in infant milk powder by HPLC-MS/MS. The sample was dissolved in water by ultrasonication, and the protein was removed by dissolving in acetonitrile. The analytes were separated on a Hypersil GOLD C₁₈ column (150 mm×2.0 mm, 5 μm) using 30 mmol/L ammonium acetate solution and methanol as mobile phases, with gradient elution at a flow rate of 0.3 mL/min. Finally, the samples were determined by HPLC-MS/MS. Internal matrix-matched calibration was used for quantification. The limits of quantification (LOQs, S/N=10) of PFOA, PFOS, BPA, and NP were 0.5, 1.0, 10.0, and 5.0 μg/kg, respectively. The recoveries ranged from 86.1% to 106.8%, and the relative standard deviations (RSDs) were in the range from 2.87% to 9.53%. The method was also applied to real samples. The results showed that the method was simple and accurate, and can be used for determining the residues of PFOA, PFOS, BPA, and NP in infant milk powder.