超声萃取-高效液相色谱法同时测定彩泥中9种防腐剂
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摘要
建立了一种同时检测彩泥制品中9种防腐剂含量(苯甲酸、苯甲醇、甲基异噻唑啉酮、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯、对羟基苯甲酸异丙酯和对羟基苯甲酸异丁酯)的超声萃取-高效液相色谱法。乙腈作为提取溶剂进行超声萃取,采用Kromasil 100-5C18色谱柱,流动相为0.05mol/L磷酸二氢钠缓冲液-甲醇-乙腈进行洗脱,流速1.5mL/min,在254nm与280nm的检测波长下35min内9种防腐剂得到良好分离。9种防腐剂检出限为5mg/kg～200mg/kg,加标回收率为90.9%～106.9%,精密度和稳定性的相对标准偏差分别为0.89%～2.88%、0.54%～2.58%。该方法简便、快速、高效、灵敏度高,为彩泥制品中多种微量防腐剂含量进行合理产品风险评估提供一种高效、可行的手段。
The nine preservatives in modeling clay included benzoic acid,benzyl alcohol,2-methyl-4-isothiazolin-3-one,methylparaben,ethylparaben,propylparaben,butylparaben,isopropylparaben and isobutylparaben.Modeling clay samples were extracted with acetonitrile in ultrasonic field.The isocratic elution was carried out on a Kromasil 100-5 C18 column,with an initial mobile phase of sodium dihydrogen phosphate buffer(0.05 mol/L)-methanol-acetonitrile,at the flow rate of 1.5 mL/min.When detector wavelength was set at 254 nm and 280 nm,the nine components were separated within 35 mins.The detection limits of those nine preservatives in modeling clay were at the range of 5-200 mg/kg.The recoveries ranged from 90.9%to 106.9%,the relative standard deviations(RSDs)of precision and stability were 0.89%-2.88%and 0.54%-2.58%,respectively.This method is efficient and feasible,can be used for the product risk assessment of trace preservatives in modeling clay.
The nine preservatives in modeling clay included benzoic acid,benzyl alcohol,2-methyl-4-isothiazolin-3-one,methylparaben,ethylparaben,propylparaben,butylparaben,isopropylparaben and isobutylparaben.Modeling clay samples were extracted with acetonitrile in ultrasonic field.The isocratic elution was carried out on a Kromasil 100-5 C18 column,with an initial mobile phase of sodium dihydrogen phosphate buffer(0.05 mol/L)-methanol-acetonitrile,at the flow rate of 1.5 mL/min.When detector wavelength was set at 254 nm and 280 nm,the nine components were separated within 35 mins.The detection limits of those nine preservatives in modeling clay were at the range of 5-200 mg/kg.The recoveries ranged from 90.9%to 106.9%,the relative standard deviations(RSDs)of precision and stability were 0.89%-2.88%and 0.54%-2.58%,respectively.This method is efficient and feasible,can be used for the product risk assessment of trace preservatives in modeling clay.
引文
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[15]钟吉强,郑荣,陈丹丹,刘畅,王柯.气相色谱-电子捕获检测器法同时检测化妆品中7个防腐剂[J].药物分析杂志,2018,38(05):806-811.
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[17]张聪,黄金凤,蔡玮红,李秀英,郭新东,何敏恒,冯翔.UPLC-MS/MS法同时测定食品接触纸包装材料中的异噻唑啉酮类和氯酚类杀菌防腐剂[J].现代食品科技,2015,31(06):303-308.
[2]彭姚珊,高俊伟,王爱霞,周天啸,刘盼,祝宁宁.高效液相色谱法测定造型黏土中2种防腐剂[J].理化检验(化学分册),2016,52(02):171-175.
[3]岳强.对羟基苯甲酸酯在人体中的暴露研究进展[J].北方环境,2011,23(03):161-165.
[4]史张欢.对羟基苯甲酸甲酯和乙酯混合暴露对雌果蝇生殖及子代的影响[D].陕西师范大学,2018.
[5]林忠洋,马万里,齐迹,李一凡.对羟基苯甲酸酯类防腐剂的人体暴露[J].化学进展,2015,27(05):614-622.
[6]李雅娟,赵晓俊,顾蔚.对羟基苯甲酸酯暴露与乳腺癌患病风险研究进展[J].卫生研究,2014,43(06):1038-1042.
[7]吕鹏,吴巍,刘丽丽,张家禹,许雷,闫艳春.甲基异噻唑啉酮对斑马鱼胚胎的急性毒性和机制研究[J].生态毒理学报,2017,12(05):260-269.
[8]QB/T 2960-2008Modeling(彩泥)[S].
[9]EN 71-9:2005+A1:2007Safety of toy-Party 9:Organic chemical compounds-requirements.
[10]2009/48/EC Directive 2009/48/EC of the European Parliament and of the council of 18June 2009on the safety of toys.
[11]严霞,曹雅军.苯甲酸在乳癖合剂中的用量与抑菌效能的研究[J].药学服务与研究,2014,14(01):79-80.
[12]牟瑞营.植物乳杆菌对奶牛乳腺炎的预防作用的研究[D].吉林大学,2017.
[13]马亚萍,徐庄剑,朱文英,胡瑜,王勍.尿样储存时间对免疫化学发光法检测促性腺激素的影响[J].中国卫生检验杂志,2014,24(22):3270-3272,3278.
[14]张倩勉,邓玉秀,刘星,刘常凯,蒋湘,李景恩,盘正华.HPLC法同时检测多种防腐剂的研究[J].食品科技,2018,43(12):341-344,348.
[15]钟吉强,郑荣,陈丹丹,刘畅,王柯.气相色谱-电子捕获检测器法同时检测化妆品中7个防腐剂[J].药物分析杂志,2018,38(05):806-811.
[16]曹淑瑞,刘治勇,张雷,李贤良,王国民,唐柏彬,袁若.高效液相色谱法同时测定食品中6种对羟基苯甲酸酯[J].分析化学,2012,40(04):529-533.
[17]张聪,黄金凤,蔡玮红,李秀英,郭新东,何敏恒,冯翔.UPLC-MS/MS法同时测定食品接触纸包装材料中的异噻唑啉酮类和氯酚类杀菌防腐剂[J].现代食品科技,2015,31(06):303-308.