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2mm的颗粒,分取1.00g,加入20mL模拟汗液或模拟唾液,浸泡2.0h后分取10mL过活化好的Oasis HLB固相萃取柱,用5mL水淋洗,8mL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2.0mL,过0.22μm滤膜。滤液进入液相色谱-串联质谱仪,目标物在AtlantisTMT3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0.1~20.0μg·L^(-1)(双酚A、双酚AF和四氯双酚A)和0.5~100.0μg·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0.3~1.5μg·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0.26~6.98mg·kg^(-1)和0.01~0.12mg·kg^(-1)。
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 0.22μm 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 0.1-20.0μg·L^(-1)(bisphenol A,bisphenol AF and tetrachlorobisphenol A)and 0.5-100.0μg·L^(-1)(other 1l phenolics),with detection limits(3S/N)in the range of 0.3-1.5μg 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.
作者
曹慧
张慧
姜侃
王瑾
杨春
CAO Hui;ZHANG Hui;JIANG Kan;WANG Jin;YANG Chun(Zhejiang Institute of Product Quality and Safety Science,Hangzhou 310018,China;Zhejiang University of Science&Technology,Hangzhou 310012,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2023年第8期883-889,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
浙江省市场监督管理局国家质量基础设施(NQI)项目(20210101、20200101)。
关键词
固相萃取
液相色谱-串联质谱法
酚类物质
儿童消费品
solid phase extraction
liquid chromatography-tandem mass spectrometry
phenolic
children consumer product
