分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
12期
1723-1728
,共6页
游钒%朱岚%何玲%冉良骥%金燕%孙成均
遊釩%硃嵐%何玲%冉良驥%金燕%孫成均
유범%주람%하령%염량기%금연%손성균
多环芳烃%代谢物%人尿液%在线固相萃取%高效液相色谱法
多環芳烴%代謝物%人尿液%在線固相萃取%高效液相色譜法
다배방경%대사물%인뇨액%재선고상췌취%고효액상색보법
Polycyclic aromatic hydrocarbon%Metabolites%Human urine%Solid phase extraction%High performance liquid chromatography
采用双三元液相色谱系统结合荧光检测器,建立了在线固相萃取-液相色谱法同时测定人尿液中7种多环芳烃代谢物的方法。目标化合物首先在Turboflow Cyclone固相萃取柱上在线富集浓缩,然后通过六通阀转移至Hypersil Green PAH色谱柱,以乙腈-水为流动相进行梯度洗脱分离,流速1.0 mL/min,柱温30℃,荧光检测器检测,分离周期为20 min。在优化的色谱条件下,5~2000 ng/L或50~20000 ng/L范围内,7种多环芳烃代谢物均呈良好的线性关系(r≥0.999),方法检出限为0.5~15 ng/L,加标回收率为80.7%~110.7%。应用本方法对吸烟和非吸烟人群尿液中7种多环芳烃代谢物的含量进行了测定,吸烟者尿液中的2-羟基萘、1-羟基萘、2-羟基菲、2-羟基芴、4-羟基菲、6-羟基显著高于非吸烟者。
採用雙三元液相色譜繫統結閤熒光檢測器,建立瞭在線固相萃取-液相色譜法同時測定人尿液中7種多環芳烴代謝物的方法。目標化閤物首先在Turboflow Cyclone固相萃取柱上在線富集濃縮,然後通過六通閥轉移至Hypersil Green PAH色譜柱,以乙腈-水為流動相進行梯度洗脫分離,流速1.0 mL/min,柱溫30℃,熒光檢測器檢測,分離週期為20 min。在優化的色譜條件下,5~2000 ng/L或50~20000 ng/L範圍內,7種多環芳烴代謝物均呈良好的線性關繫(r≥0.999),方法檢齣限為0.5~15 ng/L,加標迴收率為80.7%~110.7%。應用本方法對吸煙和非吸煙人群尿液中7種多環芳烴代謝物的含量進行瞭測定,吸煙者尿液中的2-羥基萘、1-羥基萘、2-羥基菲、2-羥基芴、4-羥基菲、6-羥基顯著高于非吸煙者。
채용쌍삼원액상색보계통결합형광검측기,건립료재선고상췌취-액상색보법동시측정인뇨액중7충다배방경대사물적방법。목표화합물수선재Turboflow Cyclone고상췌취주상재선부집농축,연후통과륙통벌전이지Hypersil Green PAH색보주,이을정-수위류동상진행제도세탈분리,류속1.0 mL/min,주온30℃,형광검측기검측,분리주기위20 min。재우화적색보조건하,5~2000 ng/L혹50~20000 ng/L범위내,7충다배방경대사물균정량호적선성관계(r≥0.999),방법검출한위0.5~15 ng/L,가표회수솔위80.7%~110.7%。응용본방법대흡연화비흡연인군뇨액중7충다배방경대사물적함량진행료측정,흡연자뇨액중적2-간기내、1-간기내、2-간기비、2-간기물、4-간기비、6-간기현저고우비흡연자。
A novel method for the simultaneous quantification of seven metabolites of polycyclic aromatic hydrocarbon in human urine was developed using online solid phase extraction-HPLC with double ternary liquid chromatography system combined with fluorescence detector. The target compounds were online concentrated on the Turboflow Cyclone solid phase extraction column at first, then transferred by the six-way valve to the Hypersil Green PAH column for separation with acetonitrile and water as mobile phase at a flow rate of 1. 0 mL/min and at 35 ℃. A single sample analysis cycle took only 20 min. Under the optimized chromatographic conditions, the method showed good linear relationship ( r≥0. 999 ) in the range of 5-2000 ng/L or 50-20000 ng/L. The LODs were 0. 5-15 ng/L, and the recoveries were 80. 7%-110. 7%. The proposed method was successfully applied in the detection of metabolites of polycyclic aromatic hydrocarbons in urine from several smokers and non-smokers. The concentrations of 2-hydroxynaphthalene, 1-hydroxynaphthalene, 2-hydroxyfluorene, 2-hydroxyphenanthrene, 4-hydroxyphenanthrene and 6-hydroxychrysene in the smokers urine were much higher than that in non-smokers.