婴幼儿奶粉中苯并[a]芘检测技术研究及含量调查  

Detection and content investigation of benzo[a]pyrene in infant milk powder

作　　者：吴平谷[1] 胡争艳[1] 王立媛[1] 王天娇[1] 马冰洁[1] 邹艳[1] 张念华[1] Wu Pinggu;Hu Zhengyan;Wang Liyuan;Wang Tianjiao;Ma Bingjie;Zou Yan;Zhang Nianhua(Zhejiang Province Center for Disease Control and Prevention,Hangzhou 310051,China)

机构地区：[1]浙江省疾病预防控制中心

出　　处：《卫生研究》2020年第1期103-106,共4页Journal of Hygiene Research

基　　金：浙江省基础公益研究计划(No.LGN19C200003);国家自然科学基金(No.31871884)

摘　　要：目的建立婴幼儿奶粉中苯并[a]芘检测技术,并对市售奶粉中苯并[a]芘含量进行调查分析。方法婴幼儿奶粉在碱性条件下用乙醚-石油醚(1∶1,V/V)提取,然后用1.5 mol/L氢氧化钾乙醇溶液皂化,固相萃取柱净化后,经DB-EUPAH色谱柱(20 m×0.18 mm×0.14μm)分离后气相色谱质谱法检测,D12-苯并[a]芘内标定量。结果当婴幼儿奶粉中苯并[a]芘加标0.3、1.0和5.0μg/kg时,平均回收率分别为116.7%、86.0%、96.4%,相对标准偏差为10.5%、4.2%和4.4%(n=6)。方法定量限为0.3μg/kg,检出限为0.1μg/kg,采用本方法对市售的40份国产及进口婴幼儿奶粉进行测定,苯并[a]芘含量范围为<0.1~0.25μg/kg,检出率为32.5%。结论本方法简便快速准确,净化效果好,灵敏度高,满足婴幼儿奶粉中苯并[a]芘检测要求。目前市售婴幼儿奶粉中苯并[a]芘含量处于较低水平。OBJECTIVE To develop a method for determination of benzo[a]pyrene and to analysis of benzo[a]pyrene content in commercially available infant milk powder.METHODS Firstly, infant milk powder was extracted with ether-petroleum ether(1∶1,V/V) under alkaline conditions, then saponified with 1.5 mol/L potassium hydroxide ethanol solution. After purification by solid phase extraction column,it was separated on DB-EUPAH chromatographic column(20 m×0.18 mm×0.14 μm) and detected by gas chromatography-mass spectrometry,and quantified using D12-benzo[a]pyrene internal standard. RESULTS When the benzo[a]pyrene in infant formula was spiked 0.3, 1.0, 5.0 μg/kg, the average recoveries were 116.7%、86.0% and 96.4%, respectively, and the relative standard deviations were 10.5%、4.2% and 4.4%, respectively(n= 6). The limit of quantification was 0.3 μg/kg, and the detection limit was 0.1 μg/kg. A total of 40 domestic and imported infant milk powders sold in Hangzhou supermarkets were analyzed. The range of benzo[a]pyrene was <0.1-0.25 μg/kg, and the detection rate was 32.5%.CONCLUSION The method has the advantages of rapid operation, good purifying effect, sensitiveness and accuracy, and meets the requirements for detection of benzo[a]pyrene in infant milk powder. The investigation reveals that the benzo[a]pyrene content in the currently marketed infant milk powder is at a low level.

关 键 词：婴幼儿奶粉 苯并[A]芘 气相色谱质谱法 食品检测 

分 类 号：R155.57[医药卫生—营养与食品卫生学] TS252.51[医药卫生—公共卫生与预防医学]