中国环境监测
中國環境鑑測
중국배경감측
ENVIRONMENTAL MONITORING IN CHINA
2014年
1期
138-143
,共6页
张盼伟%赵高峰%周怀东%余丽琴%李昆%文武%李科林
張盼偉%趙高峰%週懷東%餘麗琴%李昆%文武%李科林
장반위%조고봉%주부동%여려금%리곤%문무%리과림
药物%个人护理品%沉积物%超声萃取%高效液相色谱-串联质谱
藥物%箇人護理品%沉積物%超聲萃取%高效液相色譜-串聯質譜
약물%개인호리품%침적물%초성췌취%고효액상색보-천련질보
pharmaceutical%personal care products%sediment%ultrasonic extraction%high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS)
基于EPA1694方法,应用超声波萃取-高效液相色谱-串联质谱技术,建立了沉积物中对乙酰氨基酚、林可霉素、甲氧苄啶、咖啡因、阿奇霉素、磺胺甲唑、泰乐菌素、地尔硫卓、卡马西平及氟西汀等10种药物和个人护理品( PPCPs)的分析检测方法。样品经超声萃取、离心和SAX阴离子交换柱净化,以高效液相色谱-串联质谱仪多反应监测( MRM)模式进行离子定性、定量分析。10种药物加标回收率实验结果表明:添加低浓度样品20 ng/g,回收率为61.1%~128.5%,相对标准偏差(RSD)为1.7%~17.5%(n=5);添加高浓度样品400 ng/g,回收率为66.4%~126.7%,RSD为2.3%~18.0%(n=5),最低检测限为0.12~4.46 ng/g。该方法具有检测限低和回收率高的特点,并经实际样品验证发现,该方法适用于检测沉积物中10种PPCPs化合物。
基于EPA1694方法,應用超聲波萃取-高效液相色譜-串聯質譜技術,建立瞭沉積物中對乙酰氨基酚、林可黴素、甲氧芐啶、咖啡因、阿奇黴素、磺胺甲唑、泰樂菌素、地爾硫卓、卡馬西平及氟西汀等10種藥物和箇人護理品( PPCPs)的分析檢測方法。樣品經超聲萃取、離心和SAX陰離子交換柱淨化,以高效液相色譜-串聯質譜儀多反應鑑測( MRM)模式進行離子定性、定量分析。10種藥物加標迴收率實驗結果錶明:添加低濃度樣品20 ng/g,迴收率為61.1%~128.5%,相對標準偏差(RSD)為1.7%~17.5%(n=5);添加高濃度樣品400 ng/g,迴收率為66.4%~126.7%,RSD為2.3%~18.0%(n=5),最低檢測限為0.12~4.46 ng/g。該方法具有檢測限低和迴收率高的特點,併經實際樣品驗證髮現,該方法適用于檢測沉積物中10種PPCPs化閤物。
기우EPA1694방법,응용초성파췌취-고효액상색보-천련질보기술,건립료침적물중대을선안기분、림가매소、갑양변정、가배인、아기매소、광알갑서、태악균소、지이류탁、잡마서평급불서정등10충약물화개인호리품( PPCPs)적분석검측방법。양품경초성췌취、리심화SAX음리자교환주정화,이고효액상색보-천련질보의다반응감측( MRM)모식진행리자정성、정량분석。10충약물가표회수솔실험결과표명:첨가저농도양품20 ng/g,회수솔위61.1%~128.5%,상대표준편차(RSD)위1.7%~17.5%(n=5);첨가고농도양품400 ng/g,회수솔위66.4%~126.7%,RSD위2.3%~18.0%(n=5),최저검측한위0.12~4.46 ng/g。해방법구유검측한저화회수솔고적특점,병경실제양품험증발현,해방법괄용우검측침적물중10충PPCPs화합물。
A method for the simultaneous determination of ten pharmaceutical and personal care products ( PPCPs ) ( acetaminophen, lincomycin, trimethoprim, caffeine, azithromycin, sulfamethoxazole, tylosin, diltiazem, carbamazepine and fluoxetine) in sediments using liquid chromatography-tandem mass spectrometric was established. Samples were first extracted with ultrasonic, then cleaned up by solid phase extraction, and finally determined by tandem mass spectrometry with MRM mode. Recoveries were within 61.1%-128.5% and 66.4%-126.7% at the spiked level of 20 ng/g and 400 ng/g, respectively. The relative standard deviations (RSD, n=5) for the ten PPCPs were 1.7%-17.5% at 20 ng/g and 2.3%-18.0% at 400 ng/g. The detection limits ranged from 0.12-4.46 ng/g for ten PPCPs. The method has been successfully applied to the survey of selected ten PPCPs in sediments from Tuhai and Duliujian River, China.