气相色谱-串联质谱法测定婴幼儿配方乳粉中的丙烯酰胺

Determination of acrylamide in infant formula milk podwer by gas chromatography-tandem mass spectrometry

中文关键词:  婴幼儿配方乳粉  丙烯酰胺  气相色谱-串联质谱法

英文关键词:infant formula milk power  acrylamide  gas chromatography-tandem mass spectrometry

中文摘要:

      目的 建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定婴幼儿配方乳粉中丙烯酰胺。方法 样品经水溶解后, 用乙酸锌、亚铁氰化钾沉淀蛋白, 离心, 上清液经溴化衍生, 乙酸乙酯提取, 采用气相色谱-串联质谱法进行检测, 内标法定量。结果 丙烯酰胺在5~500 ng/mL范围内线性良好(r＞0.999), 在10、20、40 μg/kg加标浓度水平下的回收率为89.4%~107.2%, 相对标准偏差(relative standard deviations, RSDs)为3.3%~7.1% (n=6), 检出限为0.25 μg/kg, 定量限为0.75 μg/kg。结论 该方法前处理操作简便、线性良好、灵敏度高、准确度高, 抗干扰能力强, 适合婴幼儿配方乳粉中痕量丙烯酰胺的测定。

英文摘要:

      Objective To establish an analytical method for the determination of acrylamide in infant formula milk powder by gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples were dissolved in water, after the proteins were precipitated with zinc acetate and potassium ferrocyanide, centrifuged, the supernatant was brominated and then extracted with ethyl acetate, the detection was carried out by gas chromatography-tandem mass spectrometry, and the internal standard method was used for quantification. Results The linearity of acrylamide was good at 5?500 ng/mL (r>0.999). The recoveries were 89.4%?107.2% at the standard addition levels of 10, 20 and 40 μg/kg with the relative standard deviations (RSDs) in the range of 3.3%?7.1% (n=6). The limit of detection was 0.25 μg/kg, and the limit of quantification was 0.75 μg/kg. Conclusion The method has the advantages of simple pretreatment, good linearity, high sensitivity, high accuracy and strong anti-interference ability. It is suitable for the determination of trace acrylamide in infant formula milk powder.