南昌大学学报(理科版)
南昌大學學報(理科版)
남창대학학보(이과판)
JOURNAL OF NANCHANG UNIVERSITY(NATURAL SCIENCE)
2014年
1期
58-61,68
,共5页
液相色谱-串联质谱%有机锡%带鱼%超声波辅助提取%分散固相萃取
液相色譜-串聯質譜%有機錫%帶魚%超聲波輔助提取%分散固相萃取
액상색보-천련질보%유궤석%대어%초성파보조제취%분산고상췌취
Liquid chromatography-tandem mass spectrometry%Organotin compounds%Hairtail%Ultrasonic extraction%Dispersive solid-phase extraction
建立了液相色谱-串联质谱法同时测定带鱼中三甲基锡(TMT)、二苯基锡(DPhT)、二丁基锡(DBT)、三苯基锡(TPhT)和三丁基锡(TBT)分析新方法。采用 ZORBAX Eclipse plus C18色谱柱分离,以甲醇-甲酸/甲酸铵溶液(pH=2.15)为流动相,在流速0.3 mL·min-1条件下,选择梯度洗脱方式分离目标物。应用液相色谱-串联质谱仪在多重反应监测(MRM)正离子模式下进行检测。有机锡化合物在选定的浓度范围内线性关系良好,相关系数均在0.9943~0.9998之间,三甲基锡、二苯基锡、二丁基锡、三苯基锡和三丁基锡的检测限分别为300、140、140、1和1 ng·mL-1。方法回收率为64.7~96.9%,相对标准偏差为0.7~10.4%。
建立瞭液相色譜-串聯質譜法同時測定帶魚中三甲基錫(TMT)、二苯基錫(DPhT)、二丁基錫(DBT)、三苯基錫(TPhT)和三丁基錫(TBT)分析新方法。採用 ZORBAX Eclipse plus C18色譜柱分離,以甲醇-甲痠/甲痠銨溶液(pH=2.15)為流動相,在流速0.3 mL·min-1條件下,選擇梯度洗脫方式分離目標物。應用液相色譜-串聯質譜儀在多重反應鑑測(MRM)正離子模式下進行檢測。有機錫化閤物在選定的濃度範圍內線性關繫良好,相關繫數均在0.9943~0.9998之間,三甲基錫、二苯基錫、二丁基錫、三苯基錫和三丁基錫的檢測限分彆為300、140、140、1和1 ng·mL-1。方法迴收率為64.7~96.9%,相對標準偏差為0.7~10.4%。
건립료액상색보-천련질보법동시측정대어중삼갑기석(TMT)、이분기석(DPhT)、이정기석(DBT)、삼분기석(TPhT)화삼정기석(TBT)분석신방법。채용 ZORBAX Eclipse plus C18색보주분리,이갑순-갑산/갑산안용액(pH=2.15)위류동상,재류속0.3 mL·min-1조건하,선택제도세탈방식분리목표물。응용액상색보-천련질보의재다중반응감측(MRM)정리자모식하진행검측。유궤석화합물재선정적농도범위내선성관계량호,상관계수균재0.9943~0.9998지간,삼갑기석、이분기석、이정기석、삼분기석화삼정기석적검측한분별위300、140、140、1화1 ng·mL-1。방법회수솔위64.7~96.9%,상대표준편차위0.7~10.4%。
A new method was established for the simultaneous determination of trimethyltin (TMT),diphe-nyltin (DPhT),dibutyltin (DBT),triphenyltin (TPhT)and tributyltin (TBT)in hairtail by liquid chroma-tography-tandem mass spectrometry.The separation of five organotin compounds was achieved on ZORB-AX Eclipse plus C18 column with gradient elution using mixture of ammonium formate solution at pH 2.1 (adjusted with formic acid)and methanol.The flow rate was 0.3 mL/min.The detection was operated in the positive ion mode using multiple reaction monitoring.Five organotin compounds all represent good line-arity in the selected concentration range,with correlation coefficients in the range of 0.9943-0.9998.The detection limits of TMT,DPhT,DBT,TPhT and TBT were 300,140,140,1,1 ng·mL-1 ,respectively.Un-der optimized conditions,the average recoveries were ranged from 64.7% to 96.9%,with RSDs from 0.7%to 10.4%,respectively.