液质联用同时测定大鼠尿液中6种苯二氮卓类药物

建立高效液相色谱串联质谱法同时测定大鼠尿液中的6种苯二氮卓类药物(BZDs).以乙酸乙酯为萃取溶剂,经液-液萃取前处理后检测.以地西泮为内标,流动相为甲醇-0.01％甲酸+5 mmol/L甲酸铵,梯度洗脱,柱温为40℃;流速为0.3 mL/min;进样量为2 μL,质谱采用电喷雾离子源正离子模式(ESI+).8-溴-1...

Simultaneous Determination of Six Benzodiazepines in Rat Urine by Liquid Chromatography Tandem Mass Spectrometry

A liquid chromatography tandem mass spectrometry method is established for the simultaneous determination of six benzodiazepines(BZDs)in rat urine.Ethyl acetate is used as the extraction solvent,and it is tested after liquid-liquid extraction pretreatment.Diazepam is used as the internal standard,the mobile phase is methanol-(0.01% formic acid+5 mmol/L ammonium formate)with a gradient elution,the column temperature is 40℃;the flow rate is 0.3 mL/min and the injection volume is 2μL.The electrospray ion source is in positive ion mode(ESI+).The six BZDs(pyrazolam:8-bromo-1-methyl-6-pyridin-2-yl-4H-1,2,4]triazolo4,3-a]1,4]benzodiazepine;clonazepam:5-2-chlorophenyl]-l,3 dihydro-7-nitro-2H-benzodiazepin-2-one;flubromazolam:8-bromo-6-2-fluorophenyl]-1-methyl-4H-1,2,4]triazolo-4,3 a]1,4]benzodiazepine;meclonazepam:3(+)-5-(o-chlorophenyl)-1,3-dihydro-3-methyl-7-nitro-2H-1,4-benzodiazpine-2-one;flubromazepam:7-bromo-5-2-fluorophenyl]-1,3-dihydro-2H-1,4-benzodiazepin-2-one;diclazepam:7-chloro-5-2-chlorophenyl]-1-methyl-1,3-dihydro-2H-1,4-benzodiazepin-2-one)all have good linearity in the range of 20~2000 ng/mL,and the intraday and interday precisions of both 0.70%~5.60%.In the meantime,the accuracy is between 87.00% and 103.00%,and extraction recoveries of six analytes are greater than 80.00%,and the stability is good.The method is fast,simple,sensitive and accurate,which is suitable for the simultaneous measurement of the concentrations of six BZDs in rat urine.