分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
7期
1053-1056
,共4页
胡小键%张海婧%王肖红%丁昌明%金银龙%林少彬
鬍小鍵%張海婧%王肖紅%丁昌明%金銀龍%林少彬
호소건%장해청%왕초홍%정창명%금은룡%림소빈
双酚类物质%卤代双酚类物质%尿液%固相萃取%高效液相色谱串联质谱
雙酚類物質%滷代雙酚類物質%尿液%固相萃取%高效液相色譜串聯質譜
쌍분류물질%서대쌍분류물질%뇨액%고상췌취%고효액상색보천련질보
Bisphenolic compounds%Halogenatedbisphenolic compounds%Human urine%Solid phase extraction%High performance liquid chromatography-tandem mass spectrometry
建立了高效液相色谱串联质谱法同时检测人尿液中4种双酚类和卤代双酚类物质的方法。尿液样品经酶解后,采用PLEXA(亲水亲脂聚合物小柱)固相萃取柱净化,在 Atlantis? T3柱(150 mm ×3.0 mm,3μm)上,以乙腈-水为流动相,梯度洗脱,流速250μL/min,串联质谱负离子电喷雾多反应监测模式检测,基质匹配内标法定量分析。结果表明,4种物质平均回收率为86%~118.0%,日内精密度为2.6%~17.0%,日间精密度3.2%~18%,检出限为0.01~0.25μg/L。应用本方法测定200份人尿液样品,双酚A检出率为75%,检出浓度在0.58~50.5μg/L之间。本方法操作简单、灵敏、快速、可靠。
建立瞭高效液相色譜串聯質譜法同時檢測人尿液中4種雙酚類和滷代雙酚類物質的方法。尿液樣品經酶解後,採用PLEXA(親水親脂聚閤物小柱)固相萃取柱淨化,在 Atlantis? T3柱(150 mm ×3.0 mm,3μm)上,以乙腈-水為流動相,梯度洗脫,流速250μL/min,串聯質譜負離子電噴霧多反應鑑測模式檢測,基質匹配內標法定量分析。結果錶明,4種物質平均迴收率為86%~118.0%,日內精密度為2.6%~17.0%,日間精密度3.2%~18%,檢齣限為0.01~0.25μg/L。應用本方法測定200份人尿液樣品,雙酚A檢齣率為75%,檢齣濃度在0.58~50.5μg/L之間。本方法操作簡單、靈敏、快速、可靠。
건립료고효액상색보천련질보법동시검측인뇨액중4충쌍분류화서대쌍분류물질적방법。뇨액양품경매해후,채용PLEXA(친수친지취합물소주)고상췌취주정화,재 Atlantis? T3주(150 mm ×3.0 mm,3μm)상,이을정-수위류동상,제도세탈,류속250μL/min,천련질보부리자전분무다반응감측모식검측,기질필배내표법정량분석。결과표명,4충물질평균회수솔위86%~118.0%,일내정밀도위2.6%~17.0%,일간정밀도3.2%~18%,검출한위0.01~0.25μg/L。응용본방법측정200빈인뇨액양품,쌍분A검출솔위75%,검출농도재0.58~50.5μg/L지간。본방법조작간단、령민、쾌속、가고。
A method was developed for the determination of four kinds of bisphenolic and halogenated bisphenolic compounds including bisphenol F, bisphenol A, tetrachlorobisphenol A, tetrabromobisphenol A in human urine using high performance liquid chromatography-tandem mass spectrometry. The analytes was extracted by solid phase extraction. The separation of the analytes was achieved on an Atlantis T3 column (3. 0×150 mm, 3 μm) gradient eluted with the mobile phase of acetonitrile and water at the rate of 250 μL/min, and detected by an electrospray ionization tandem mass spectrometry in the multiple-reaction-monitoring negative mode. The quantification was carried out by matrix-matched calibration curve. The average recoveries at 3 spiked levels were 86%-118%, with intra-day precision of 2 . 6%-17 . 0% and inter-day precision of 3. 2%-18. 0%. The limits of detection of four analytes (S/N=3) were 0. 01-0. 25 μg/L. The method was applied to the analysis of 200 human urines samples and the results showed that the method was simple, sensitive and reliable.