摘要
建立了非那西丁的气相色谱/质谱/质谱(GC/MS/MS)联用检测血中去痛片的主要代谢物非那西丁的新方法。采用液液提取法,用乙醚提取血中非那西丁,提取物水浴浓缩后进行GC/MS和GC/MS/MS分析,检测总离子流色谱(TIC)和一级质谱,并以非那西丁一级质谱基峰为母离子的测定其二级质谱,体内药物用GC/MS全扫描定性分析即用二级质谱结合其总离子流色谱峰的保留时间定性;选择离子扫描定量分析,采用内标曲线法,根据非那西丁和内标SKF525A二级质谱的TIC峰面积比进行定量分析。
A new method was developed for the analysis of 2,6-diethylaniline（2,6-DEA）, the major metabolite of alachor, in urine by heptafluorobutyryl （HFB） derivatization-gas chromatography/tandem mass spectrometry（GC/MS/MS）. After urine samples were extracted with cyclohexane, the extracts were derivatized with heptafluorobutyrylchloride （ HFBC） , and then the total ion chromagrams（ TIC） , mass spectra and tandem mass spectra of derivatives were acquired. 2 ,6-DEA was identified by the tandem mass spectra and the retention time of its TIC chromatograms. Using 2 , 5-dichloroaniline as the internal standard, quantification was performed according to the peak area ratio of the TIC peak from tandem mass spectrometry of the derivatives of 2 ,6-DEA and internal standard. The internal standard calibration curve of 2 ,6 DEA derivative was used in quantification. The method was sensitivity and accurate for the qualitative and quantitative analysis of 2 ,6-DEA in urine samples. The extraction efficiency of 2 ,6-DEA was 96. 2%. The limit of detection and the limit of quantization were 2. 0 ng/mL and 6. 6 ng/mL respectively. The repeatability was good that RSD was 4. 72%. The accuracy was high that relative recoveries were 99. 0%. Using this method, the urine samples of the rabbit’s ingested alachor were measured and the results showed that the method can be applied to the forensic identification.
出处
《广州化工》
CAS
2014年第24期108-110,共3页
GuangZhou Chemical Industry
关键词
非那西丁
血
气相色谱/质谱联用
2,6-diethylaniline
gas chromatography/tandem mass spectrometry
heptafluorobutyryl derivatization
urine
