通过式固相萃取-气相色谱-三重四极杆串联质谱法同时测定淡水鱼中14种麻醉剂的残留量

Simultaneous Determination of Residues of 14 Anesthetics in Freshwater Fish by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry with Pass-Through Solid Phase Extraction

提出了通过式固相萃取-气相色谱-三重四极杆串联质谱法(GC-MS/MS)同时测定淡水鱼中丁香酚、甲基丁香酚、异丁香酚、顺式-甲基异丁香酚、乙酸丁香酚酯、乙酰基异丁香酚、丙泊酚、三卡因、苯佐卡因、利多卡因、普鲁卡因、普莫卡因、丁卡因和布他卡因等14种麻醉剂残留量的方法。称取处理好的样品2 g,加入5.00 mg·L^(-1)内标溶液100μL和水5 mL,涡旋混匀,静置30 min。加入乙腈10 mL提取,再加入氯化钠2 g盐析分层,离心,取5 mL上清液加载到PRiME HLB柱上,收集流出液。取2 mL流出液,加入二甲基亚砜50μL,常温下氮吹至近干,用丙酮1.0 mL复溶,经0.22μm微孔滤膜过滤,滤液供GC-MS/MS测定。采用HP-5MS UI毛细管色谱柱分离各目标物,以电子轰击离子源和多反应监测模式检测,内标法定量。结果表明:14种麻醉剂工作曲线的线性范围为0.005~0.400 mg·L^(-1),检出限为0.001 mg·kg^(-1);以阴性样品为基质进行3个浓度水平的加标回收试验,日内、日间回收率为75.3%~120%,日内、日间精密度(n=6)为1.3%~10%;方法用于33份实际样品分析,有15份样品中检出丁香酚,检出量为0.0136~0.462 mg·kg^(-1)。

A method for the determination of residues of 14 anesthetics,including eugenol,methyleugenol,isoeugenol,cis-methyl isoeugenol,eugenyl acetate,acetyl isoeugenol,propofol,tricaine,benzocaine,lidocaine,procaine,pramoxine,tetracaine and butacaine,in freshwater fish by gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS)with pass-through solid phase extraction was proposed.The processed sample(2 g)was taken,and 100μL of 5.00 mg·L^(-1) internal standard solution and 5 mL of water were added.The mixture was mixed well by vortex,and settled for 30 min.Acetonitrile(10 mL)was added into above mixture for extraction,and 2 g of sodium chloride was added for salting out stratification.After centrifugation,5 mL of the supernatant was loaded onto PRiME HLB column,and the effluent was collected.An aliquot(2 mL)was taken,and 50μL of dimethyl sulfoxide was added.The solution was blown to nearly dryness at room temperature by nitrogen.Then the residue was redissolved with 1.0 mL of acetone,and filtered by 0.22μm microporous membrane.The filtrate was determined by GC-MS/MS.HP-5 MS UI capillary column was used to separate target compounds,and electron impact ion source and multiple reaction monitoring mode were used for detection,with internal standard method for quantification.It was shown that the linear ranges of working curves of 14 anesthetics were 0.005-0.400 mg·L^(-1),with the same detection limits of 0.001 mg·kg^(-1).Test for recovery was made on negative sample as matrix at 3 concentration levels by addition standard method,giving values of recovery of intra-day and inter-day were in the range of 75.3%-120%,and precision(n=6)of intra-day and inter-day were in the range of 1.3%-10%.This method was applied to the analysis of 33 actual samples,and eugenol was detected in 15 samples,with detection amounts in the range of 0.0136-0.462 mg·kg^(-1).