分析化学
分析化學
분석화학
Chinese Journal of Analytical Chemistry
2015年
11期
1743-1748
,共6页
王春蕾%刘华良%马永建%阮丽萍
王春蕾%劉華良%馬永建%阮麗萍
왕춘뢰%류화량%마영건%원려평
在线固相萃取%多环芳烃%高效液相色谱%食用油
在線固相萃取%多環芳烴%高效液相色譜%食用油
재선고상췌취%다배방경%고효액상색보%식용유
Online solid phase extraction%Polycyclic aromatic hydrocarbons high performance liquid chromatography%Edible oil
建立了植物油中15+1种欧盟优控多环芳烃的在线固相萃取-高效液相色谱-紫外/荧光( online-SPE-HPLC-UV/FLD)检测分析方法。食用油样品经异丙醇稀释定容并过滤,固相萃取柱ChromSpher Pi (80 mm×3 mm)在线净化,反相C18 PAH专用柱(250 mm×4.6 mm i. d,5μm)分离,异丙醇、乙腈和水为流动相,梯度洗脱,紫外(220 nm)和荧光检测器检测。结果表明,15+1种多环芳烃在相应的线性范围内峰面积与质量浓度之间线性良好(R2>0.99);检出限为0.03~12.23μg/kg;3个水平加标回收率为65.3%~110.5%;相对标准偏差为0.1%~9.8%。
建立瞭植物油中15+1種歐盟優控多環芳烴的在線固相萃取-高效液相色譜-紫外/熒光( online-SPE-HPLC-UV/FLD)檢測分析方法。食用油樣品經異丙醇稀釋定容併過濾,固相萃取柱ChromSpher Pi (80 mm×3 mm)在線淨化,反相C18 PAH專用柱(250 mm×4.6 mm i. d,5μm)分離,異丙醇、乙腈和水為流動相,梯度洗脫,紫外(220 nm)和熒光檢測器檢測。結果錶明,15+1種多環芳烴在相應的線性範圍內峰麵積與質量濃度之間線性良好(R2>0.99);檢齣限為0.03~12.23μg/kg;3箇水平加標迴收率為65.3%~110.5%;相對標準偏差為0.1%~9.8%。
건립료식물유중15+1충구맹우공다배방경적재선고상췌취-고효액상색보-자외/형광( online-SPE-HPLC-UV/FLD)검측분석방법。식용유양품경이병순희석정용병과려,고상췌취주ChromSpher Pi (80 mm×3 mm)재선정화,반상C18 PAH전용주(250 mm×4.6 mm i. d,5μm)분리,이병순、을정화수위류동상,제도세탈,자외(220 nm)화형광검측기검측。결과표명,15+1충다배방경재상응적선성범위내봉면적여질량농도지간선성량호(R2>0.99);검출한위0.03~12.23μg/kg;3개수평가표회수솔위65.3%~110.5%;상대표준편차위0.1%~9.8%。
A novel method was developed for the determination of the 15+1 European priority polycyclic aromatic hydrocarbons in edible oil by online solid-phase extraction coupled with high performance liquid chromatography-ultraviolet/ fluorescence detection ( online-SPE-HPLC-UV/FL-D ) . The edible oil samples were diluted with isopropyl alcohol, and then filtered. The online extraction was performed on a solid phase extraction ChromSpher Pi column (80 mmí3 mm) and the separation was carried out on a C18 reversed-phase PAH column (250 mmí4. 6 mm i. d, 5μm) using ultraviolet detection at 220 nm and fluorescence detection. Isopropyl alcohol, acetonitrile and water were served as mobile phase in gradient elution. The results showed good linearity for the 15+1 polycyclic aromatic hydrocarbons with all the correlation coefficients (R2)>0. 99. The limits of detection ( LODs ) were between 0. 03 and 12. 23 μg/kg. The recoveries of the sixteen components in the three levels of spiked samples were in the range of 65 . 3%-110 . 5% with the relative standard deviation (RSD, n=6) from 0. 1% to 9. 8%.