大体积进样气质联用法检测涉水产品浸泡液中的酚类物质  

Determination of Phenols in Soak Water from Drinking Water Related Products by Gas Chromatography-Mass Spectrometry with Large Volume Injection

作　　者：徐小民[1,2] 朱岩[2] 李蕊[3] 宋国良[1] 韩见龙[1] 赵永信[1] 应英[1] 冯靓[1] 张念华[1] 任一平[1] 

机构地区：[1]浙江省疾病预防控制中心,杭州310051 [2]浙江大学化学系,杭州310028 [3]温州医学院,温州325035

出　　处：《分析化学》2011年第2期253-256,共4页Chinese Journal of Analytical Chemistry

基　　金：浙江省分析测试科技计划(No.2008F70002);浙江省医学重点学科群建设计划(No.XKQ-009-003)资助项目

摘　　要：建立了涉水产品浸泡液中酚类物质的柱头大体积进样(OCI-LVI)、串联毛细管柱分离、气相色谱-质谱联用(GC-MS)定性与定量检测方法。样品按相关法规浸泡后,以0.2 g/L的比例立即加入还原剂Na2S2O3,以消除过量余氯。取10 mL浸泡液,加入2,4-二溴酚内标物质,调pH 6.8,NaCl饱和后加1 mL提取溶剂提取,静置分层,取上清液30μL进样。考察了OCI-LVI-GC-MS法中,极性串联短柱(聚乙二醇柱)在增强挥发性组分色谱保留能力方面的作用。方法的检出限(LODs)为0.1～1μg/L;回收率为76.7%～112%;相对标准偏差(RSD)为5.94%～12.4%。其中的挥发酚类LODs远低于相关卫生标准(2μg/L)。A method was developed for the determination of phenols in soak water from drinking water related products by gas chromatography-mass spectrometry（GC-MS） with on-column large volume injection（OCI-LVI） and coupled column separation.The sample was firstly soaked according to related standard method.And then,0.2 g/L of Na2S2O3 was used as reductant to remove excessive chlorine.After spiked 2,4-dibromo-phenol as internal standard,10 mL of the soak water was adjusted to pH 6.8,saturated by NaCl and extracted by 1 mL of organic solvent.Approximately 30 μL of up-layer extract was used as injecting sample.The advantage of the short coupled polar column in increasing retention capacity of volatile phenols in OCI-GC-MS system was discussed.The LODs were 0.1-1 μg/L.The recoveries were 76.7%-112% with 5.94%-12.4% of RSD.

关 键 词：柱头大体积进样 气相色谱-质谱联用 串联毛细管柱 涉水产品 酚类 

分 类 号：O657.63[理学—分析化学]