ASE_GC_MS法同时测定海洋沉积物中65种多氯联苯_多环芳烃与有机氯农药

第30卷第2期分析测试学报Vol 30No 2

2011年2月FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)152~160

ASE/GC-MS法同时测定海洋沉积物中65种

多氯联苯、多环芳烃与有机氯农药

贺行良

青岛 266071;

1,2,3

,夏 宁,张媛媛,王江涛

1,223

(1.国土资源部海洋油气资源与环境地质重点实验室,山东 青岛 266071;2.青岛海洋地质研究所,山东

3.中国海洋大学 海洋化学理论与工程技术教育部重点实验室,山东 青岛 266100)

摘 要:建立了加速溶剂萃取/气相色谱-质谱法(ASE/GC-MS)同时测定海洋沉积物中28种多氯联苯(PCBs)、16种多环芳烃(PAHs)和21种有机氯农药(OCPs)的分析方法。结果表明,ASE的最佳萃取温度为100 ,最佳静态时间为5min。GC-MS同时分析65种化合物时,线性系数(r2)为0 991~0 999;

PAHs的线性范围为0 05~5 00mg/L,

r2不低于0 996。PCBs、

PCBs和OCPs的线性范围为5 0~500 0 g/L,

PAHs和OCPs的检出限分别为0 03~0 11、0 04~0 73、0 06~0 48 g/kg,定量下限分别为0 11~0 35、0 12~2 42、0 18~1 61 g/kg,平均加标回收率为70%~146%,方法的相对标准偏差(n=6)为1 2%~17 3%。经海洋沉积物标准参考物质验证,该方法高效、准确,适合海洋沉积物中65种化合物的同时定量分析。

关键词:海洋沉积物;多氯联苯;多环芳烃;有机氯农药;同时测定

中图分类号:O657 63;F767 2 文献标识码:A 文章编号:1004-4957(2011)02-0152-09do:i10 3969/j issn 1004-4957 2011 02 007

SimultaneousDeterminationof65PolychlorinatedBiphenyls,Polycyclic

AromaticHydrocarbonsandOrganochlorinePesticidesinMarineSedimentsbyGC-MSwithAcceleratedSolventExtraction

HEXing liang

1,2,3

,XIANing,ZHANGYuan yuan,WANGJiang tao

1,223

(1.KeyLaboratoryofMarineHydrocarbonResourcesandEnvironmentalGeology,MinistryofLandandResources,

Qingdao 266071,China;

2.QingdaoInstituteofMarineGeology,Qingdao 266071,China;3.Key

ofChina,Qingdao 266100,

China)

LaboratoryofMarineChemistryTheoryandTechnology,MinistryofEducation,OceanUniversity

Abstrac:tAgaschromatography-massspectrometry(GC-MS)coupledwithacceleratedsolventextraction(ASE)methodwasdevelopedforthesimultaneousdeterminationof28polychlorinatedbi phenyls,16polycyclicaromatichydrocarbonsand21organochlorinepesticidesinmarinesediments.Theresultsindicatedthatthebestsimultaneousextractiontemperatureandtimewere100 and

5min,respectively.Undertheoptimalconditions,theanalysisof65compoundswerecarriedoutwithGC-MS.Thecalibrationcurveswerelinearintherangeof0 05-5 00mg/LforPAHswithcorrelationcoefficients(r)of0 991-0 999and5 0-500 0 g/LforPCBsandOCPswithrnolessthan0 996.ThelimitsofdetectionofPCBs,PAHsandOCPswereintherangeof0 03-0 11,0 04-0 73,0 06-0 48 g/kg,andthelimitsofquantitationwereintherangeof0 11-0 35,0 12-2 42,0 18-1 61 g/kg,respectively.Thespikedrecoveriesrangedfrom70%

to

146%withRSDs(n=6)of1 2%-17 3%forallthecompounds.Throughmarinesedimentsstand ardreferencematerials,themethodwasprovedtobeeffectiveandaccurate,andcouldbeappliedinthesimultaneousdeterminationof65compoundsinmarinesediments.Keywords:marinesediments;ganochlorinepesticides;

polychlorinatedbiphenyls;

polycyclicaromatichydrocarbons;

or

simultaneousdetermination

2

2

收稿日期:2010-10-08;修回日期:2010-11-03

基金项目:国土资源部海洋油气资源与环境地质重点实验室基金资助项目(RME200918)通讯作者:贺行良,Te:l0532-85755845,

E-mai:lqdhxl2008@126 com