Determination of 14 Phenolics Migration in Children Consumer Products by Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction
摘 要
儿童通过手、口等途径接触儿童消费品时,双酚A等酚类物质会通过唾液或汗液迁移到体内,影响儿童健康,而关于唾液和汗液中酚类物质迁移量检测的报道较少,因此进行了题示研究。将样品剪碎或粉碎成粒径小于2 mm的颗粒,分取1.00 g,加入20 mL模拟汗液或模拟唾液,浸泡2.0 h后分取10 mL过活化好的Oasis HLB固相萃取柱,用5 mL水淋洗,8 mL甲醇洗脱。收集洗脱液,氮吹至近干,用30%(体积分数)甲醇溶液稀释至2.0 mL,过0.22 μm滤膜。滤液进入液相色谱-串联质谱仪,目标物在AtlantisTM T3色谱柱上以不同体积比的水和体积比1∶1的甲醇-乙腈混合溶液进行梯度洗脱分离,以电喷雾离子源负离子模式电离,以多反应监测模式检测,以基质匹配法定量。结果显示:14种酚类物质的质量浓度分别在0.1~20.0 μg·L-1(双酚A、双酚AF和四氯双酚A)和0.5~100.0 μg·L-1(其他11种酚类物质)内与峰面积呈线性关系,检出限(3S/N)为0.3~1.5 μg·kg-1。按标准加入法进行回收试验,模拟汗液和模拟唾液中14种酚类物质的回收率分别为82.5%~106%和80.5%~108%,测定值的相对标准偏差(n=5)分别为0.40%~9.1%和0.30%~8.7%。方法用于6份双酚A和壬基酚阳性样品的分析,双酚A和壬基酚的迁移量分别为0.26~6.98 mg·kg-1和0.01~0.12 mg·kg-1。
Abstract
When children came into contact with children consumer products through their hands and mouth, phenolics such as bisphenol A would migrate into the body through saliva or sweat, affecting children health. However, there were few reports on the detection of phenolics migration in saliva and sweat, so research mentioned by the title was conducted. The samples were cut or crushed into particles with diameter smaller than 2 mm, and an aliquot (1.00 g) was mixed with 20 mL of simulated sweat or simulated saliva for soaking for 2.0 h. An aliquot (10 mL) was passed through the Oasis HLB solid phase extraction column activated beforehand, then the column was rinsed with 5 mL of water, and eluted with 8 mL of methanol. The eluate was collected, blown to near dryness by nitrogen, diluted to 2.0 mL with 30% (volume fraction) methanol solution, and passed through a 0.22 μm filter membrane, and the filtrate was introduced into the liquid chromatograph-tandem mass spectrometer. Targets were separated on the AtlantisTM T3 chromatographic column with mixed solutions composed of methanol-acetonitrile mixed solution at volume ratio of 1:1 and water at different volume ratios by gradient elution, ionized by the negative ion mode of the electric spray ion source, detected by the multiple reaction monitoring mode, and quantified by the matrix matching method. As found by the results, linear relationships between values of the mass concentration and the peak area of 14 phenolics were kept in the ranges of 0.1-20.0 μg·L-1 (bisphenol A, bisphenol AF and tetrachlorobisphenol A) and 0.5-100.0 μ g·L-1 (other 11 phenolics), with detection limits (3S/N) in the range of 0.3-1.5 μg·kg-1. Test for recovery was made according to standard addition method, giving recoveries of 14 phenolics in the ranges of 82.5%-106% in simulated sweat and 80.5%-108% in simulated saliva, respectively. RSDs (n=5) of the determined values were in the ranges of 0.40%-9.1% and 0.30%-8.7%, respectively. The proposed method was applied to the analysis of 6 positive samples of bisphenol A and nonylphenol, with migration amounts of bisphenol A and nonylphenol in the ranges of 0.26-6.98 mg·kg-1 and 0.01-0.12 mg·kg-1, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202308003
所属栏目 工作简报
基金项目 浙江省市场监督管理局国家质量基础设施(NQI)项目(20210101、20200101)
收稿日期 2021/10/21
修改稿日期
网络出版日期
作者单位点击查看
备注曹慧,高级工程师,博士,主要从事质谱分析工作,1248547195@qq.com
引用该论文: CAO Hui,ZHANG Hui,JIANG Kan,WANG Jin,YANG Chun. Determination of 14 Phenolics Migration in Children Consumer Products by Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(8): 883~889
曹慧,张慧,姜侃,王瑾,杨春. 固相萃取-液相色谱-串联质谱法测定儿童消费品中14种酚类物质的迁移量[J]. 理化检验-化学分册, 2023, 59(8): 883~889
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参考文献
【1】艾舜豪,李霁,王晓南,等.太湖双酚A的水质基准研究及风险评价[J].环境科学研究, 2020,33(3):581-588.
【2】王艳婷,于学燕,姚蓉,等.食品接触材料中双酚A迁移与检测的研究进展[J].食品研究与开发, 2017,38(22):219-224.
【3】贾聪聪,刘丽艳,王亚文,等.紫外分光光度法测定热敏纸中的双酚S[J].河北大学学报(自然科学版), 2020,40(2):144-150.
【4】陈荣祥,王莉,王杰,等.高效液相色谱法测定食品包装材料中双酚A的含量[J].理化检验-化学分册, 2017,53(10):1167-1170.
【5】刘丽艳,白洁,王亚文,等.高效液相色谱法测定厨房用纸中双酚S[J].理化检验-化学分册, 2019,55(5):584-590.
【6】黄会,邓旭修,张华威,等.凝胶渗透色谱-固相萃取-气相色谱-质谱法测定水产品中辛基酚、壬基酚和双酚A[J].食品科学, 2013,34(24):116-120.
【7】JUREK A, LEITNER E. Analytical determination of bisphenol A (BPA) and bisphenol analogues in paper products by GC-MS/MS[J]. Food Additives & Contaminants:Part A, 2017,34(7):1225-1238.
【8】JUREK A, LEITNER E. Analytical determination of bisphenol A (BPA) and bisphenol analogues in paper products by LC-MS/MS[J]. Food Additives & Contaminants:Part A, 2018,35(11):2256-2269.
【9】郭项雨,李海玉,吕庆,等.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.
【10】乔玲,凌睿,胡文彦,等.食品中双酚A等3种酚类物质含量测定[J].食品研究与开发, 2014,35(17):97-99.
【11】张品,张晶,陈洁君,等.在线固相萃取-超高效液相色谱-串联质谱法测定乳制品中双酚A等4种内分泌干扰物[J].分析化学, 2014,42(12):1811-1817.
【12】陈龙星,李昆,花中霞,等.塑料包装调味品中双酚A的高效液相色谱-串联质谱测定法[J].环境与健康杂志, 2019,36(5):451-453.
【13】华永有,林麒,卢翠英.全自动固相萃取-超高效液相色谱-串联质谱法同时测定江水中8种酚类内分泌干扰物[J].理化检验-化学分册, 2019,55(8):904-911.
【14】丁洁,张圣虎,刘济宁,等.液相色谱-串联质谱法测定污水处理厂水样中双酚A、四溴双酚A及烷基酚类化合物[J].色谱, 2014,32(5):529-534.
【15】张明,唐访良,徐建芬,等.UPLC-MS/MS法同时测定地表水中6种双酚类化合物残留[J].质谱学报, 2017,38(6):690-698.
【16】马强,白桦,王超,等.液相色谱-串联质谱法同时测定纺织品和食品包装材料中的壬基酚、辛基酚和双酚A[J].分析化学, 2010,38(2):197-201.
【17】张圣虎,张易曦,吉贵祥,等.高效液相色谱-串联质谱法测定儿童和成人尿液中双酚A、四溴双酚A和辛基酚[J].分析化学, 2016,44(1):19-24.
【18】梁锡镇,隋海霞,李丹,等.液相色谱-三重四极杆质谱同时测定食品接触材料中双酚A、双酚F与双酚S的迁移量[J].分析测试学报, 2018,37(1):87-91.
【19】谢景千,杨俊,黎永乐.液相色谱-串联质谱法测定食品接触材料中双酚F和双酚S的迁移量[J].食品安全质量检测学报, 2020,11(24):9100-9107.
【20】熊小婷,王继才,王海洋,等.RRLC-MS/MS同时测定食品接触材料中9种双酚类化合物迁移量[J].质谱学报, 2019,40(2):151-158.
【2】王艳婷,于学燕,姚蓉,等.食品接触材料中双酚A迁移与检测的研究进展[J].食品研究与开发, 2017,38(22):219-224.
【3】贾聪聪,刘丽艳,王亚文,等.紫外分光光度法测定热敏纸中的双酚S[J].河北大学学报(自然科学版), 2020,40(2):144-150.
【4】陈荣祥,王莉,王杰,等.高效液相色谱法测定食品包装材料中双酚A的含量[J].理化检验-化学分册, 2017,53(10):1167-1170.
【5】刘丽艳,白洁,王亚文,等.高效液相色谱法测定厨房用纸中双酚S[J].理化检验-化学分册, 2019,55(5):584-590.
【6】黄会,邓旭修,张华威,等.凝胶渗透色谱-固相萃取-气相色谱-质谱法测定水产品中辛基酚、壬基酚和双酚A[J].食品科学, 2013,34(24):116-120.
【7】JUREK A, LEITNER E. Analytical determination of bisphenol A (BPA) and bisphenol analogues in paper products by GC-MS/MS[J]. Food Additives & Contaminants:Part A, 2017,34(7):1225-1238.
【8】JUREK A, LEITNER E. Analytical determination of bisphenol A (BPA) and bisphenol analogues in paper products by LC-MS/MS[J]. Food Additives & Contaminants:Part A, 2018,35(11):2256-2269.
【9】郭项雨,李海玉,吕庆,等.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.
【10】乔玲,凌睿,胡文彦,等.食品中双酚A等3种酚类物质含量测定[J].食品研究与开发, 2014,35(17):97-99.
【11】张品,张晶,陈洁君,等.在线固相萃取-超高效液相色谱-串联质谱法测定乳制品中双酚A等4种内分泌干扰物[J].分析化学, 2014,42(12):1811-1817.
【12】陈龙星,李昆,花中霞,等.塑料包装调味品中双酚A的高效液相色谱-串联质谱测定法[J].环境与健康杂志, 2019,36(5):451-453.
【13】华永有,林麒,卢翠英.全自动固相萃取-超高效液相色谱-串联质谱法同时测定江水中8种酚类内分泌干扰物[J].理化检验-化学分册, 2019,55(8):904-911.
【14】丁洁,张圣虎,刘济宁,等.液相色谱-串联质谱法测定污水处理厂水样中双酚A、四溴双酚A及烷基酚类化合物[J].色谱, 2014,32(5):529-534.
【15】张明,唐访良,徐建芬,等.UPLC-MS/MS法同时测定地表水中6种双酚类化合物残留[J].质谱学报, 2017,38(6):690-698.
【16】马强,白桦,王超,等.液相色谱-串联质谱法同时测定纺织品和食品包装材料中的壬基酚、辛基酚和双酚A[J].分析化学, 2010,38(2):197-201.
【17】张圣虎,张易曦,吉贵祥,等.高效液相色谱-串联质谱法测定儿童和成人尿液中双酚A、四溴双酚A和辛基酚[J].分析化学, 2016,44(1):19-24.
【18】梁锡镇,隋海霞,李丹,等.液相色谱-三重四极杆质谱同时测定食品接触材料中双酚A、双酚F与双酚S的迁移量[J].分析测试学报, 2018,37(1):87-91.
【19】谢景千,杨俊,黎永乐.液相色谱-串联质谱法测定食品接触材料中双酚F和双酚S的迁移量[J].食品安全质量检测学报, 2020,11(24):9100-9107.
【20】熊小婷,王继才,王海洋,等.RRLC-MS/MS同时测定食品接触材料中9种双酚类化合物迁移量[J].质谱学报, 2019,40(2):151-158.
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