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时间:2020-04-20
《气相色谱法测定贻贝中的多氯联苯和有机氯农药.pdf》由会员上传分享,免费在线阅读,更多相关内容在行业资料-天天文库。
1、第42卷第l4期广州化工Vo1.42No.142014年7月GuangzhouChemicalIndustryJu1.2014气相色谱法测定贻贝中的多氯联苯和有机氯农药冰孙秀梅,胡红美,钟志,金衍健,陈雪昌,何依娜,郭远明(浙江省海洋水产研究所,浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江舟山316012)摘要:建立了贻贝中多氯联苯和有机氯农药的超声提取固相萃取净化气相色谱检测方法,以正己烷一二氯甲烷作为溶剂进行超声提取,提取液经浓硫酸溶液和硅胶一弗罗里土固相萃取柱净化,再采用GC—ECD进行分析。本方法采用外标法进行定量分析,在2.5~100g/L浓度范围内,相关系数r2>0.99
2、51;多氯联苯和有机氯农药的检出限分别在0.01~0.04g/kg和0.039~0.24g/kg;各组分加标回收率在75%一115%之间(n=6),RSD<15%。方法简便快速、重现性高,检测灵敏度和准确度均满足贻贝中多氯联苯和有机氯农药分析的要求。关键词:超声提取;固相萃取净化;气相色谱法;多氯联苯;有机氯农药;贻贝中图分类号:0657.15文献标志码:A文章编号:1001—9677(2014)014—0134—04DeterminationofP0lychl0rinatedBiphenylsandorgan0chl0rinatedPesticidesinMusselbyGasChroma
3、tographySUNXiu—mei,HUHong—mei,ZHONGZhi,JINYah-jian,CHENXue—chang,HEYi—na,GUOYuan—ming(MarineFisheryInstituteofZhejingProvince,KeyLaboratoryofSustainableUtilizationofTechnologyResearchforFisheryResourceofZhejiangProvince,ZhejiangZhoushan316012,China)Abstract:Agaschromatographymethodwasdevelopedandva
4、lidatedfordeterminationofpolychlorinatedbiphenyls(PCBs)andorganochlorinatedpesticides(OPCs)inmusselbasedonultrasonic—assistedextractionandsolidphaseextractionasaclean—upprocedure.Thebiologicalsampleswereextractedultrasonicallywithhexane,andtreatedwithsulfuricacid.f01lowedbyclean—upwithsolidphaseext
5、ractioncolumncontaininoctadecylsilicagelandflorisil.Themethodrealizedcompletebase—lineseparationofthePCBsandOPCsandhighsensitivedeterminationbasedOiloptimizationofgaschromatographicconditions,thetemperatureprogramandselectedionmonitoring.Underoptimizingconditions,thedetectionlimitsforPCBsandOCPswer
6、e0.O1—0.04g/kgand0.039~0.241xg/kg,respectively,thecalibrationcurvesofthePCBsandOPCswere1inearintherangeof2.5—100ug/Lwithcorrelationcoemcientsnotlessthan0.995.Therecoveriesatthespikedamountof1.0kg,10.0kgand100.0g/kgwere75%~115%(RSD<15%).Thereproducible,sensitiveandaccuratemethodwassuitableforquality
7、controlofthePCBsandOCPsinmusse1.Keywords:ultrasonicextraction;solidphaseextractionclean—up;gaschromatography;polychlorinatedbiphenyls;organochlorinatedpesticides;mussel持久性有机污染物中的多氯联苯(PCBs)和有机氯农药2000ng/g(湿质量
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