第32卷，第3期2023年3月化学分析计量CHEMICALANALYSISANDMETERAGEVol.32,No.3Mar.2023顶空气相色谱法同时测定生活饮用水中17种挥发性卤代烃刘晓晶，张媛媛，平小红，华正罡，曹忠波（辽宁省疾病预防控制中心，沈阳110172）摘要建立了顶空气相色谱法同时测定生活饮用水中17种挥发性卤代烃的分析方法。样品采用自动顶空进样技术，经DB–5毛细管色谱柱（30m×0.32mm，0.25μm）分离后，用电子捕获检测器检测。优化样品保存条件为加入0.5g抗坏血酸，冷藏避光保存。优化顶空条件：平衡温度为70℃，平衡时间为30min，NaCl添加量为2.5g。使用4-溴氟苯作为质控物质，保证测定结果的准确性。17种挥发性卤代烃的标准曲线相关系数均不小于0.998，方法检出限为0.003～2μg/L，平均回收率为85.7%～105.7%，测定结果的相对标准偏差为1.0%～5.6%（n=6）。该方法快速、灵敏度高、重现性好，适用于生活饮用水中17种挥发性卤代烃的同时测定。关键词生活饮用水；顶空；气相色谱法；挥发性卤代烃中图分类号：O657.7文献标识码：A文章编号：1008-6145(2023)03-0050-06Simultaneousdeterminationof17kindsofvolatilehalogenatedhydrocarbonsindrinkingwaterbyheadspacegaschromatographyLIUXiaojing,ZHANGYuanyuan,PINGXiaohong,HUAZhenggang,CAOZhongbo(CenterforDiseaseControlandPreventionofLiaoningProvince，Shengyang110172，China)AbstractAmethodwasestablishedforthesimultaneousdeterminationof17volatilehalogenatedhydrocarbonsindrinkingwaterbyheadspacegaschromatography.Thesampleswereinjectedbyautomaticheadspacesamplingtechnology,separatedbyDB-5capillarycolumn(30m×0.32mm,0.25μm),andanalyzedbyECDdetector.Optimizesamplestorageconditionswereadded0.5gascorbicacid,refrigeratedandprotectedfromlight.Optimizeheadspaceconditionswereequilibriumtemperatureof70℃,equilibriumtimeof30min,NaCladditionof2.5g.4-bromofluorobenzenewasusedasqualitycontrolmaterialtoensuretheaccuracyofdetermination.Thestandardcurvecorrelationcoefficientsof17volatilehalogenatedhydrocarbonswereallnotlessthan0.998.Thedetectionlimitsofthemethodwerewithin0.003-2μg/L,theaveragerecoveryrateswerewithin85.7%-105.7%,andtherelativestandarddeviationsofdeterminationresultswerewithin1.0%-5.6%(n=6).Thismethodisrapid,sensitiveandrepeat...
