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1、第42卷第13期廣州化工Vol_42No.132014年7月GuangzhouChemicalIndustryJu1.2014.-_I-.-L-'!同效液相色譜一熒光檢測(cè)法測(cè)定貝類中15種多環(huán)芳烴孫秀梅,胡紅美,梅光明,陳雪昌,郭遠(yuǎn)明(浙江省海洋水產(chǎn)研究所,農(nóng)業(yè)部漁業(yè)環(huán)境及水產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)測(cè)試中心,浙江省海洋漁業(yè)資源可持續(xù)利用技術(shù)研究重點(diǎn)實(shí)驗(yàn)室,浙江舟山316012)摘要:建立了高效液相色譜一程序熒光檢測(cè)法同時(shí)測(cè)定貝類中15種多環(huán)芳烴的方法。通過液相色譜柱、熒光激發(fā)和發(fā)射波長(zhǎng)等條件的優(yōu)化,實(shí)現(xiàn)15種多環(huán)芳烴組分基線完全分離和熒光高靈敏度檢測(cè)。在優(yōu)化的實(shí)驗(yàn)條件下,檢測(cè)
2、的15種多環(huán)芳烴中萘、苊和芴的檢出限為0.5Ixg/kg,苯并[b]熒蒽、二苯并[a,h]蒽和苯并[g,h,i]茈的檢出限為2.0Ixg/kg,其余化合物的檢出限為1.0Ixs/kg;在檢測(cè)的15種多環(huán)芳烴中,菲、葸、芘、苯并[a]蒽、崩、苯并[a]芘、茚并[1,2,3一cd]芘在0.001~0.5mg/L濃度范圍,其余化合物在0.002~1.0mg/L濃度范圍,呈良好的線性相關(guān),相關(guān)系數(shù)r>0.995;當(dāng)樣品加標(biāo)水平分別為2、10、100g/kg時(shí),回收率在71.1%~98.4%,RSD<10%。該檢測(cè)方法重現(xiàn)性高,檢測(cè)靈敏度和準(zhǔn)確度均滿足分析要求。關(guān)鍵詞:多環(huán)芳烴
3、;貝類;高效液相色譜;熒光法中圖分類號(hào):065文獻(xiàn)標(biāo)志碼:A文章編號(hào):1001—9677(2014)013—0123—04Determinationof15PolycyclicAromaticHydr0carb0nsinShellfishbyHPLC—-FLDSUNXiu—mei,HUHong—mei,MEIGuang—ming,CHENXue—chang,GUOYuan—ming(MarineFisheryInstituteofZhejiangProvince,F(xiàn)isheryEnvironmentandAquaticProductsQualitySupervisio
4、nTestingCenter,KeyLaboratoryofSustainableUtilizationofTechnologyResearchforFisheryResourceofZhejiangProvince,ZhejiangZhoushan316012,China)Abstract:Highperformanceliquidchromatography(HPLC)coupledtoafluorescencedetector(FLD)wasusedtosetupananalyticalprocedureforthequantificationof15EUpri
5、oritypolycyclicaromatichydrocarbons(PAHs)inaquaticproducts.Themethodrealizedthecompletebase—lineseparationof15PAHsandhighsensitiveflurescencedeterminationafteroptimizinganalyticalconditions,includingliquidchromatographicconditions,excitationandemissionwavelength.Undertheoptimizedconditi
6、ons,thedetectionlimitsofnaphthalene,acenaphtheneandfluorenewere0.5kg,thedetectionlimitsofbenzo(b)fluoranthene,dibenzo(a,h)anthraceneandbenzo(g,h,i)perylenewere2.0kg,thedetectionlimitsoftheotherswere1.0g/kg.The15PAHshadgoodlinearity(r>0.995),intherangeof0.001~0.5mg/L.Therecoveriesatthesp
7、ikedamountof2,10,and100g/kg,respectively,were71.1%~98.4%,andtheRSDswerelessthan10%.Themethodishighlysensitiveandaccurate.Itcanbeusedforthequalitycontrolof15PAHsinmanyaquaticproducts.Keywords:polycyclicaromatichydrocarbons;aquaticproducts;highperformanceliquidchromatography;fluo