气相色谱-串联质谱法测定婴儿奶粉中16种邻苯二甲酸酯类化合物

doi:10.3724/SP.J.1123.2018.03010

色谱 ›› 2018, Vol. 36 ›› Issue (8): 786-794.DOI: 10.3724/SP.J.1123.2018.03010

气相色谱-串联质谱法测定婴儿奶粉中16种邻苯二甲酸酯类化合物

许兵兵^1,2, 李晓敏², 张庆合², 朱维晃¹

1. 西安建筑科技大学环境与市政工程学院, 陕西西安 710055;
2. 中国计量科学研究院化学计量与分析科学研究所, 北京 100029

收稿日期:2018-03-08 出版日期:2018-08-08 发布日期:2014-06-28
通讯作者: 李晓敏,Tel:(010)64524784,E-mail:lixm@nim.ac.cn;朱维晃,E-mail:zhuweihuang@gmail.com
基金资助:
中国计量科学研究院基本科研业务费专项（21-AKY1619）.

Determination of 16 phthalate acid esters in infant formula by gas chromatography-tandem mass spectrometry

XU Bingbing^1,2, LI Xiaomin², ZHANG Qinghe², ZHU Weihuang¹

1. School of Environmental and Municipal Engineering, Xi'an University of Architecture & Technology, Xi'an 710055, China;
2. Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, China

Received:2018-03-08 Online:2018-08-08 Published:2014-06-28
Supported by:
Financing Funding of National Institute of Metrology, China (No.21-AKY1619).

摘要/Abstract

摘要：

建立了气相色谱-串联质谱（GC-MS/MS）测定复杂基体婴儿奶粉中16种邻苯二甲酸酯类塑化剂的分析方法。奶粉样品以水溶解均质，乙腈提取，乙二胺-N-丙基硅烷（PSA）类型玻璃固相萃取柱净化，DB-5 MS UI气相色谱柱（30 m×0.25 mm×0.25 μm）分离，同位素稀释质谱法（IDMS）定量。比较了氧化铝/PSA和PSA两种固相萃取柱在不同洗脱条件下萃取16种塑化剂的回收率。最终选择PSA固相萃取柱，以正己烷-丙酮（60：40，v/v）作为洗脱溶剂，实现奶粉基体中16种塑化剂的净化。采用基质匹配同位素内标法定量，16种塑化剂在0.01~2.0 mg/kg范围内线性良好，线性相关系数（R²）大于0.9996，检出限和定量限分别是0.15~2.50 μg/kg和0.50~8.33 μg/kg，加标回收率为96.1%~104.0%，相对标准偏差（RSD）小于3.3%（n=5），该方法灵敏度好、精密度高，适用于婴儿奶粉基体中16种塑化剂的痕量分析。

关键词: 固相萃取, 邻苯二甲酸酯类塑化剂, 气相色谱-串联质谱, 同位素稀释质谱法, 婴儿奶粉

Abstract:

A method was established for the determination of 16 phthalate acid esters (PAEs) in infant formula by gas chromatography-tandem mass spectrometry (GC-MS/MS). PAEs in infant formula samples were homogenized by deionized water, extracted with acetonitrile, and purified by a solid-phase extraction (SPE) method using primary secondary amine (PSA) sorbents. The separation was performed on a DB-5 MS UI (30 m×0.25 mm×0.25 μm) capillary column. Effects of different elution solvents on alumina/PSA and PSA SPE columns were investigated. Fair recoveries of 16 PAEs were achieved on the PSA column upon elution by mixed n-hexane-acetone (60:40, v/v). All the 16 PAEs were quantified by matrix-matched isotopic-dilution mass spectrometry (IDMS); the 16 PAEs showed linear relationships in the concentration range of 0.01-2.0 mg/kg with linear coefficients (R²) greater than 0.9996. The limits of detection (LODs) and quantification (LOQs) were in the range of 0.15-2.5 μg/kg and 0.50-8.33 μg/kg, respectively. The recoveries of the 16 PAEs, obtained using the IDMS method, were 96.1%-104.0% with relative standard deviations (RSDs) lower than 3.3% (n=5). These results established the method described here as sensitive and precise for the simultaneous determination of 16 PAEs in infant formula, even at trace concentrations.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), infant formula, isotopic-dilution mass spectrometry (IDMS), phthalate acid esters (PAEs), solid-phase extraction (SPE)

中图分类号:

O658

许兵兵, 李晓敏, 张庆合, 朱维晃. 气相色谱-串联质谱法测定婴儿奶粉中16种邻苯二甲酸酯类化合物[J]. 色谱, 2018, 36(8): 786-794.

XU Bingbing, LI Xiaomin, ZHANG Qinghe, ZHU Weihuang. Determination of 16 phthalate acid esters in infant formula by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(8): 786-794.

参考文献

[1] Staples C A, Peterson D R, Parkerton T F, et al. Chemosphere, 1997, 35(4):667
[2] Bo Y N, Li R, Zhang P J, et al. Chinese Journal of Chromatography, 2016, 34(9):868 薄艳娜, 李蓉, 张朋杰, 等. 色谱, 2016, 34(9):868
[3] Afshari A, Gunnarsen L, Clausen P A, et al. Indoor Air, 2004, 14(2):120
[4] Wang W L, Wu Q Y, Wang C, et al. Environ Sci Pollut Res, 2015, 22(5):3620
[5] Zeng F, Cui K, Xie Z, et al. J Hazard Master, 2009, 164(2/3):1171
[6] Mankidy R, Wiseman S, Ma H, et al. Toxicol Lett, 2013, 217(1):50
[7] Lópezcarrillo L, Hernándezramírez R U, Calafat A M, et al. Environ Health Perspect, 2010, 118(4):539
[8] Zhang J, Chen H M. Modern Chemical Industry, 2011, 31(12):1 张静, 陈会明. 现代化工, 2011, 31(12):1
[9] European Food Safety Authority. Opinion of the Scientific Panel on Food Additives, Flavourings, Processing Aids and Material in Contact with Food on a Request from the Commission related to Di-butyl Phthalate (DBP) for Use in Food Contact Materials.[2018-03-08]. https://www.efsa.europa.eu/en/efsajournal/pub/242
[10] European Food Safety Authority. Opinion of the Scientific Panel on Food Additives, Flavourings, Processing Aids and Material in Contact with Food on a Request from the Commission Related to Butylbenzyl Phthalate (BBP) for Use in Food Contact Materials.[2018-03-08]. https://www.efsa.europa.eu/en/efsajournal/pub/241
[11] European Food Safety Authority. Opinion of the Scientific Panel on Food Additives, Flavourings, Processing Aids and Material in Contact with Food on a Request from the Commission related to Bis(2-ethylhexyl) Phthalate (DEHP) for Use in Food Contact Materials.[2018-03-08]. https://www.efsa.europa.eu/en/efsajournal/pub/243
[12] Yano K, Hirosawa N, Sakamoto Y, et al. Bull Environ Contam Toxicol, 2005, 74(2):373
[13] Fierens T, Van H M, Willems H, et al. Food Chem Toxicol, 2012, 50(8):2945
[14] Lin J, Chen W, Zhu H, et al. J Dairy Sci, 2015, 98(12):8278
[15] Cao X L. Compr Rev Food Sci Food Saf, 2010, 9(1):21
[16] Fierens T, Holderbeke M V, Willems H, et al. Environ Int, 2013, 51(5):1
[17] Liu N Y, Xia M, Wang H M, et al. Food and Nutriton in China, 2013, 19(4):70 刘宁玉, 厦明, 王慧铭, 等. 中国食物与营养, 2013, 19(4):70
[18] Russo M V, Avino P, Perugini L, et al. Rsc Adv, 2015, 5(46):37023
[19] Yue M E, Xu J, Hou W G. J Anal Chem, 2015, 70(9):1147
[20] Farajzadeh M A, Djozan D, Mogaddam M R, et al. J Sep Sci, 2012, 35(5/6):742
[21] Miclean M, Cadar O, Roman C. Stud Univ Babes-Bolyai Chem, 2012, 57(1):127
[22] Du Z N, Miao H J, Wu Y N, et al. Journal of Hygiene Research, 2016, 45(3):465 杜珍妮, 苗宏健, 吴永宁, 等. 卫生研究, 2016, 45(3):465
[23] Ren R, Jin Q, He H L, et al. Chromatographia, 2016, 79(13/14):903
[24] Guo Y, Kannan K. Anal Bioanal Chem, 2012, 404(9):2539
[25] Li Z K, Xu L G, Peng C F, et al. J Chromatogr Sci, 2011, 49(4):338
[26] Guo J, Ma J, Liu S, et al. Acta Scientiae Circumstantiae, 2006, 26(1):111 郭瑾, 马军, 刘嵩, 等. 环境科学学报, 2006, 26(1):111
[27] Xia B, Liu Y B, Ren Z, et al. Chinese Journal of Health Laboratory Technology, 2015, 25(19):6 夏冰, 刘玉波, 任峥, 等. 中国卫生检验杂志, 2015, 25(19):6
[28] Zhang M M, Liu Y L, Ma Y X, et al. China Oils and Fats, 2015, 40(2):56 张明明, 刘玉兰, 马宇翔, 等. 中国油脂, 2015, 40(2):56
[29] Wang J, Li X M, Zhang Q H, et al. J Sep Sci, 2015, 38(10):1700
[30] Huang Y H. Food Research and Development, 2010, 31(11):167 黄永辉. 食品研究与开发, 2010, 31(11):167
[31] He J, Lv R, Zhu J, et al. Anal Chim Acta, 2010, 661(2):215
[32] Shaikh H, Memon N, Khan H, et al. J Chromatogr A, 2012, 1247(14):125
[33] Stanislaw W, Dariusz D, Roman K. J Chromatogr A, 2015, 1412:22

气相色谱-串联质谱法测定婴儿奶粉中16种邻苯二甲酸酯类化合物

Determination of 16 phthalate acid esters in infant formula by gas chromatography-tandem mass spectrometry

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