杭州市售婴幼儿配方乳粉中16种欧盟优控多环芳烃的表征及调查分析

Characterization and investigation of 16 European priority polycyclic aromatic hydrocarbons in commercial infant formula milk powder in Hangzhou

目的建立婴幼儿配方乳粉中16种欧盟优控多环芳烃的气相色谱质谱测定方法,并对2020年70份杭州市售的国内外配方乳粉中16种欧盟优控多环芳烃进行表征及调查分析。方法婴幼儿配方乳粉经水解、提取、皂化及固相萃取柱净化,用DB-EUPAH毛细管柱(20 m×0.18 mm,0.14μm)分离后,气相色谱质谱法检测,内标法定量。结果婴幼儿配方乳粉中16种欧盟优控多环芳烃加标0.5~5.0μg/kg时,平均回收率为67.8%~116.2%,相对标准偏差为2.0%~15.1%(n=6),方法的定量限为0.5μg/kg,检出限为0.2μg/kg。采用本法对市售的70份婴幼儿配方乳粉进行测定,16种欧盟优控多环芳烃的含量范围为<0.2~0.48μg/kg,其中PAH4的含量范围为<0.2~0.91μg/kg,调查检出的婴幼儿配方乳粉中16种欧盟优控多环芳烃主要是■、环戊并[c,d]芘、苯并[a]蒽、苯并[b]荧蒽、苯并[g,h,i]苝。结论本方法简便、准确,适合婴幼儿配方乳粉中16种欧盟优控多环芳烃的检测,监测结果表明杭州市售的婴幼儿配方乳粉中欧盟优控多环芳烃含量较低,均符合欧盟的限量要求。

OBJECTIVE A gas chromatography-mass spectrometry(GC-MS)method for the determination of 16 European priority polycyclic aromatic hydrocarbons(16 EUPAHs)in infant formula milk powder was established,and the characterization and investigation of 16 EUPAHs in 70 milk formula powders were carried out in 2020.METHODS After hydrolysis,extraction,saponification and solid phase extraction,infant formula milk powder was detected by GC-MS using DB-EUPAH capillary column(20 m×0.18 mm,0.14μm)and quantified by internal standard method.RESULTS The average recoveries ranged from 67.8%to 116.2%and the relative standard deviations ranged from 2.0%to 15.1%(n=6).The limits of quantification and detection of the method were 0.5 and 0.2μg/kg,respectively.The content of 16 EUPAHs was<0.2-0.48μg/kg,including PAH4 content in the range of<0.2-0.91μg/kg,the characterization and investigation of infant formula powder in 16 EUPAHs mainly chrysene,cyclopenta[c,d]pyrene,benz[a]anthracene,benzo[b]fluoranthene,benzo[g,h,i]perylene.CONCLUSION The method is simple,accurate and suitable for the determination of 16 EUPAHs in infant formula milk powder.The result showed that the content of 16 EUPAHs in commercially available infant formula milk powder in Hangzhou was low and all of them met the limit requirement of European Union.