Simultaneous Determination of 5 Phenolic Endocrine Disruptors in Toys by LC-MS/MS
摘 要
采用液相色谱-串联质谱法测定玩具中5种酚类内分泌干扰物(即双酚A、对叔辛基酚、邻正壬基酚、对正辛基酚及对正壬基酚的含量)。ABS塑料玩具样品以四氢呋喃为提取溶剂,超声辅助溶解,用甲醇沉淀塑料基质;布绒玩具样品用甲醇作为提取溶剂,超声提取。提取液采用Waters XBridge C18色谱柱分离,以不同比例的甲醇和0.1%(体积分数)氨水溶液的混合液作为流动相进行梯度洗脱,洗脱液供质谱分析,质谱测定中选择电喷雾负离子源和多反应监测模式。5种化合物的质量浓度在一定范围内与峰面积呈线性关系,上述5种酚类化合物的测定下限(10S/N)分别为1.0,1.0,1.0,0.5,0.5 μg·kg-1。加标回收率在87.4%~105%之间,测定值的相对标准偏差(n=6)均小于9.1%。
Abstract
LC-MS/MS was applied to the determination of 5 phenolic endocrine disruptors (i.e. bisphenol A, 2-octylphenol, 2-nonylphenol, 4-n-octylphenol and 4-n-nonylphenol) in toys. For ABS plastic toys, the sample was ultrasonically extracted with tetrahydrofuran and then the plastic matrix was separated by precipitation with methanol. For cloth fabric toys, the sample was ultrasonically extracted with methanol, and the extract was separated on Waters XBridge C18 column, using a mixture of methanol and (φ) 0.1% ammonia solution (mixed in various ratio) as mobile phase in the gradient elution. ESI- and MRM were adopted in MS. Linear relationships were found between values of peak areas and mass concentrations of the 5 phenolic endocrine disruptors in definite ranges. The lower limits of determinaiton (10S/N) for the above mentioned phenols were 1.0, 1.0, 1.0, 0.5, 0.5 μg·kg-1 respectively. Values of recovery obtained by standard addition method were in the range of 87.4%-105%, with RSDs (n=6) were less than 9.1%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201512017
所属栏目 工作简报
基金项目 “双打”中玩具有机类有害物质检验鉴定方法研究 (2012104018-12);塑胶和木制儿童用品中典型环境激素迁移规律 研究(201310057)。
收稿日期 2014/11/25
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备注郭项雨(1986-),男,北京人,工程师,硕士,主要研 究方向为工业与消费品安全及检测技术。
引用该论文: GUO Xiang-yu,LI Hai-yu,LV Qing,ZHANG Qing,LI Pi,BAI Hua,WANG Zhi-juan,WANG Wan. Simultaneous Determination of 5 Phenolic Endocrine Disruptors in Toys by LC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(12): 1708~1712
郭项雨,李海玉,吕庆,张庆,李丕,白桦,王志娟,王婉. 液相色谱-串联质谱法同时测定玩具中5种酚类内分泌干扰物[J]. 理化检验-化学分册, 2015, 51(12): 1708~1712
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参考文献
【1】张慧珠.内分泌干扰物生物检测研究进展[J].环境科学导刊, 2014,33(增1):8-15.
【2】马莉,史乾涛,袁小英,等.内分泌干扰物对鲤鱼器官中离子平衡的影响[J].环境化学, 2014,33(3):381-385.
【3】王国华,云霞,那广水,等.海洋生物组织中酚类内分泌干扰物分析方法的建立与应用[J].海洋环境科学, 2014,33(1):89-98.
【4】朱毅,舒为群,田怀军,等.辛基酚体外类雌激素效应观察[J].第三军医大学学报, 2003,25(8):673-375.
【5】肖晶.双酚A和烷基酚的检测与暴露评估[D].北京:中国疾病预防控制中心, 2008.
【6】REACH (2006) Registration, Evaluation, Authorization and Restriction of Chemicals[S].
【7】Directive 2009/48/EC of EUropean Parliament on the Safety of toy[S].
【8】Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 Establishing a Framework for Community Action in the Field of Water Policy[S].
【9】肖晶,邵兵,吴永宁,等.HPLC-FL法检测尿液中类雌激素双酚A和烷基酚[J].中国食品卫生杂志, 2008,20(2):111-114.
【10】徐靖,刘娟,金江岚,等.分子印迹基质固相分散-超高效液相色谱法测定儿童玩具中双酚A[J].理化检验-化学分册, 2011,47(6):665-671.
【11】BABAY P A, GETTAR R T, SILVA M F, et al. Separation of nonylpenol ethoxylates and nontlpjenol by non-aqueous capillary electrophoresis[J]. J Chromatogr A, 2006,1116(12):277-285.
【12】吴婷妮.毛细管电泳技术在中药酚类活性成分中的应用研究[D].合肥:安徽医科大学, 2012.
【13】邵敏,董锁拽,王敏.红外光谱对纺织助剂中烷基酚聚氧乙烯醚的快速定性和定量[J].纺织学报, 2014,35(6):80-84.
【14】高永刚,张艳艳,高建国,等.衍生化气相色谱-质谱法测定玩具和食品接触材料中双酚A[J].色谱, 2012,30(10):1017-1020.
【15】张岩,马晓斐,吕品,等.液相色谱-串联质谱法测定小型家用电器塑料部件中双酚A[J].色谱, 2012,30(1):95-98.
【16】俞雪钧,谷云云,冯睿,等.高效液相色谱-串联质谱法同时测定海产品中双酚A及烷基酚残留[J].华中农业大学学报, 2014,33(3):52-59.
【17】LU Qing, ZHANG Qing, LI Wen-tao, et al. Determination of 48 fragrance allergensin toys using GC with ion trap MS/MS[J]. J Separation Science, 2013,36:3534-3549.
【18】孙银峰,牛增元,叶曦雯,等.液相色谱-质谱法测定电气产品塑料部件中的初级芳香胺[J].分析化学, 2009,37(6):861-866.
【19】李金玲,黄理纳,刘华鼐,等.液相色谱-串联质谱联用法测定玩具材料中的双酚A[J].广东化工, 2013,40(12):172-173.
【20】李海玉,白桦,吕庆,等.布绒玩具中致敏性芳香物质的快速筛查方法研究[J].分析化学, 2013,41(10):1518-1525.
【2】马莉,史乾涛,袁小英,等.内分泌干扰物对鲤鱼器官中离子平衡的影响[J].环境化学, 2014,33(3):381-385.
【3】王国华,云霞,那广水,等.海洋生物组织中酚类内分泌干扰物分析方法的建立与应用[J].海洋环境科学, 2014,33(1):89-98.
【4】朱毅,舒为群,田怀军,等.辛基酚体外类雌激素效应观察[J].第三军医大学学报, 2003,25(8):673-375.
【5】肖晶.双酚A和烷基酚的检测与暴露评估[D].北京:中国疾病预防控制中心, 2008.
【6】REACH (2006) Registration, Evaluation, Authorization and Restriction of Chemicals[S].
【7】Directive 2009/48/EC of EUropean Parliament on the Safety of toy[S].
【8】Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 Establishing a Framework for Community Action in the Field of Water Policy[S].
【9】肖晶,邵兵,吴永宁,等.HPLC-FL法检测尿液中类雌激素双酚A和烷基酚[J].中国食品卫生杂志, 2008,20(2):111-114.
【10】徐靖,刘娟,金江岚,等.分子印迹基质固相分散-超高效液相色谱法测定儿童玩具中双酚A[J].理化检验-化学分册, 2011,47(6):665-671.
【11】BABAY P A, GETTAR R T, SILVA M F, et al. Separation of nonylpenol ethoxylates and nontlpjenol by non-aqueous capillary electrophoresis[J]. J Chromatogr A, 2006,1116(12):277-285.
【12】吴婷妮.毛细管电泳技术在中药酚类活性成分中的应用研究[D].合肥:安徽医科大学, 2012.
【13】邵敏,董锁拽,王敏.红外光谱对纺织助剂中烷基酚聚氧乙烯醚的快速定性和定量[J].纺织学报, 2014,35(6):80-84.
【14】高永刚,张艳艳,高建国,等.衍生化气相色谱-质谱法测定玩具和食品接触材料中双酚A[J].色谱, 2012,30(10):1017-1020.
【15】张岩,马晓斐,吕品,等.液相色谱-串联质谱法测定小型家用电器塑料部件中双酚A[J].色谱, 2012,30(1):95-98.
【16】俞雪钧,谷云云,冯睿,等.高效液相色谱-串联质谱法同时测定海产品中双酚A及烷基酚残留[J].华中农业大学学报, 2014,33(3):52-59.
【17】LU Qing, ZHANG Qing, LI Wen-tao, et al. Determination of 48 fragrance allergensin toys using GC with ion trap MS/MS[J]. J Separation Science, 2013,36:3534-3549.
【18】孙银峰,牛增元,叶曦雯,等.液相色谱-质谱法测定电气产品塑料部件中的初级芳香胺[J].分析化学, 2009,37(6):861-866.
【19】李金玲,黄理纳,刘华鼐,等.液相色谱-串联质谱联用法测定玩具材料中的双酚A[J].广东化工, 2013,40(12):172-173.
【20】李海玉,白桦,吕庆,等.布绒玩具中致敏性芳香物质的快速筛查方法研究[J].分析化学, 2013,41(10):1518-1525.
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