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.
Wei Sheng Yan Jiu. 2020 Jan;49(1):103-106. doi: 10.19813/j.cnki.weishengyanjiu.2020.01.018.
To develop a method for determination of benzo[a]pyrene and to analysis of benzo[a]pyrene content in commercially available infant milk powder.
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 D_(12)-benzo[a]pyrene internal standard.
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%.
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.
建立测定苯并[a]芘的方法，并分析市售婴儿奶粉中苯并[a]芘的含量。
首先，在碱性条件下用乙醚 - 石油醚（1∶1，V/V）提取婴儿奶粉，然后用1.5 mol/L氢氧化钾乙醇溶液皂化。经固相萃取柱净化后，在DB - EUPAH色谱柱（20 m×0.18 mm×0.14 μm）上分离，采用气相色谱 - 质谱联用仪检测，并用D_(12)-苯并[a]芘内标进行定量。
婴儿配方奶粉中苯并[a]芘的加标量为0.3、1.0、5.0 μg/kg时，平均回收率分别为116.7%、86.0%和96.4%，相对标准偏差分别为10.5%、4.2%和4.4%（n = 6）。定量限为0.3 μg/kg，检出限为0.1 μg/kg。对杭州超市销售的40种国产和进口婴儿奶粉进行了分析。苯并[a]芘含量范围为<0.1 - 0.25 μg/kg，检出率为32.5%。
该方法具有操作快速、净化效果好、灵敏准确等优点，符合婴儿奶粉中苯并[a]芘检测要求。调查显示，目前市售婴儿奶粉中苯并[a]芘含量处于较低水平。
