邻苯二甲酸酯类标准物质在婴幼儿乳粉塑化剂检测中的应用研究

doi:10.7538/tws.2020.33.05.0279

摘要/Abstract

摘要：

采用自行研制的6种氘标记邻苯二甲酸酯做内标，对婴幼儿乳粉中16种邻苯二甲酸酯进行测定。乳粉中加入一定量氘标记邻苯二甲酸酯后采用超纯水溶解，利用正己烷进行提取，采用气相色谱-质谱联用仪在选择离子模式下进行分析，内标法定量。16种邻苯二甲酸酯在0.02 μg/mL~1.0 μg/mL范围内线性关系良好，相关系数均大于0.999。基质空白加标在0.05 μg/mL~1.0 μg/mL范围内时回收率为90.8%~103.6%，相对偏差为0.51%~3.75%。同位素内标的使用消除了基质效应对检测产生的影响，提高了检测方法的回收率，有效避免痕量检测中假阳性现象的发生。

关键词: 氘标记邻苯二甲酸酯, 婴幼儿乳粉, 塑化剂, 检测

Abstract:

Infant milk powder is the main dietary nutrition source for infants except breast milk, and its product quality directly affects infant development. Sixteen phthalates in infant milk powder were determined by using six deuterium labeled phthalates as internal standard. After a certain amount of deuterium was added into the milk powder, phthalate was dissolved in ultra-pure water, extracted with hexane, analyzed with gas chromatography-mass spectrometry and determined with internal standard method. The linear relationship of 16 phthalates was good in the range of 0.02 μg/mL to 1.0 μg/mL, and the correlation coefficients were all greater than 0.999. The recovery was 90.8%-103.6% in the range of 0.05 μg/mL-1.0 μg/mL and the relative deviation was 0.51%-3.75%. The effect of matrix effect on detection is eliminated and the recovery of detection method is improved.

Key words: deuterium labeled phthalate, infant milk powder, plasticizer, detection

孙雯;李杰;杜晓宁;徐仲杰;潘洁;尤雅芳;李美华. 邻苯二甲酸酯类标准物质在婴幼儿乳粉塑化剂检测中的应用研究[J]. 同位素, 2020, 33(5): 279-285.

SUN Wen;LI Jie;DU Xiaoning;XU Zhongjie;PAN Jie;YOU Yafang;LI Meihua. Study on the Application of Phthalate Esters in The Detection of Plasticizer in Infant Milk Powder[J]. Journal of Isotopes, 2020, 33(5): 279-285.

参考文献

［1］王守法,周耀武,宁啸骏，等. 气相色谱-质谱法测定婴幼儿乳粉中16种邻苯二甲酸酯类迁移物［J］. 包装与食品机械,2013,31(6):61-64.Wang Shoufa, Zhou Yaobin, Ning Xiaojun, et al. Determination of 16 Phthalate Esters Migrants Content in Infant Milk Powder by GC-MS［J］. Packaging and Food Machinery, 2013, 31(6): 61-64（in Chinese）.
［2］郑宏儒,徐雪霏,李春阳,等. 吉林省婴幼儿食品中邻苯二甲酸酯类塑化剂含量检测［J］. 食品安全导刊,2020:99-100.Zheng Hongru, Xu Xuefei, Li Chunyang, et al. Detection of Phthalate plasticizer in infant food in Jilin Province［J］. Guide to Food Safety, 2020: 99-100（in Chinese）.
［3］陈鑫兰,项林敏,李娜,等. 食品接触材料中邻苯二甲酸酯类增塑剂含量测定与微波条件下的迁移研究［J］. 农产品加工,2019(12):56-59.Chen Xinlan, Xiang Linmin, LI Na, et al. Detection of Phthalate Acid Esters Content in Food Contact Materials and Study on Migration of Microwave Conditions［J］. Farm Products Processing, 2019(12): 56-59（in Chinese）.
［4］中华人民共和国国家卫生和计划生育委员会，国家食品药品监督管理总局. GB 5009.271—2016 食品安全国家标准《食品中邻苯二甲酸酯的测定》［S］. 北京:中国标准出版社，2016.
［5］任民红,左海根,曾海龙,等. 气质联用法测定白酒中邻苯二甲酸二丁酯的不确定度评定［J］. 酿酒科技,2015(1):111-114.Ren Minhong, Zuo Haigen, Zeng Hailong, et al. Evaluation of the uncertainties in the determination of D ibutyl phthalate in baijiu (Liquor)by GC-MS［J］.Liquor-Making Science & Technology, 2015(1): 111-114（in Chinese）.
［6］王佳敏,邹海民,王希希,等. 分散液液微萃取-气相色谱/质谱法测定松茸中18种邻苯二甲酸酯［J］. 现代预防医学,2020,47(7):1291-1295.Wang Jiamin, Zou Haimin, Wang Xixi, et al. Determination of 18 phthalate acid esters in matsutake by dispersiveliquid liquid microextraction-gas chromatography/mass spectrometry［J］. Modern Preventive Medicine, 2020, 47(7): 1291-1295（in Chinese）.
［7］张少倩. 固相萃取-气相色谱法测定水中邻苯二甲酸酯类化合物［J］. 化学工程师,2019(12):29-31.Zhang Shaoqian. Determination of phthalates esters in water by SPE coupled with gas chromatography［J］. Chemical Engineer, 2019(12): 29-31(in Chinese).
［8］彭文浩,沈平. 气质联用法快速检测白酒中的邻苯二甲酸酯类物质［J］. 中国卫生检验杂质,2019,29(17):2 068-2070.Peng Wenhao, Shen Ping. Rapid determination of phthalate esters in liquorsby gas chromatography-mass spectrometry［J］. Chin J Health Lab Tec, 2019, 29(17): 2068-2070（in Chinese）.
［9］张清,龙梅,吴荣荣,等. 儿童玩具中邻苯二甲酸酯类塑化剂含量分析［J］. 研究与开发,2020,46(4):175-184.Zhang Qing, Long Mei, Wu Rongrong, et al. Analysis on the content of phthalates plasticizer in children’s toys［J］. Research and Development, 2020, 46(4): 175-184（in Chinese）.
［10］张瑶,马桂娟,冯秀娟. 气相色谱-质谱联用对枸杞籽油中塑化剂迁移量的研究［J］. 食品研究与开发,2020,41(4):179-184.Zhagn Yao, Ma Guijuan, Feng Xiujuan. The investigation of plasticizers migration volume in the boxthorn seed oil by gas chromatography-Mass spectrometry［J］. Food Research And Development, 2020, 41(4): 179-184（in Chinese）.

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