QTRAP LC-MS/MS法检测血、尿中莫达非尼

Determination of Modafi nil in Blood and Urine by QTRAP LC-MS/MS

本文采用超高效液相色谱-四级杆/线性离子阱质谱技术,建立血液、尿液中莫达非尼的检测方法。选取卡马西平为内标,血液、尿液经甲醇/乙腈(体积比1︰1)混合提取剂提取,高速离心,取上清液过滤膜,以0.1%(体积分数)甲酸/水溶液和0.1%(体积分数)甲酸/乙腈作为流动相,经Phenomenex Kinetex~?C18(2.1mm×100 mm×2.6μm)色谱柱分离,以电喷雾正离子多反应监测-信息依赖性采集-增强离子扫描(MRMIDA-EPI),结合二级谱库检索进行分析。结果显示,莫达非尼在1~80 ng/mL范围内线性关系良好,线性相关系数大于0.997;血液、尿液方法检出限(S/N≥3)均为0.5 ng/mL,定量限(S/N≥10)均为0.8 ng/mL;2、20、80 ng/mL低、中、高添加浓度水平血液、尿液回收率分别为80.1%~110.3%、87.9%~109.1%,相对标准偏差均小于10%。此方法可满足实际办案中对莫达非尼滥用者血液、尿液的定性定量分析。

In this paper,a method for the determination of modafinil in blood and urine was established by ultraperformance liquid chromatography-tandem hybrid-quadrupole-linear ion trap mass spectrometry.Carbamazepine was selected as the internal standard,and blood and urine were extracted with methanol/acetonitrile(V/V,1︰1),then centrifuged at high speed,and filtrated by membrane.Using 0.1%(V/V)formic acid/water solution and 0.1%(V/V)formic acid/acetonitrile as mobile phase,the mixture was separated on Phenomenex Kinetex C18(2.1 cm×100 mm×2.6μm)column.Electrospray positive ion monitoring/information-dependent collection/enhanced ion scanning(MRM-IDA-EPI)and secondary library retrieval were used for analysis.In the range of 1-80 ng/mL,modafinil had a good linear relationship,and the linear correlation coefficient was greater than 0.997.The limit of detection(S/N≥3)of blood and urine was 0.5 ng/mL,and the lower limit of quantifation(S/N≥10)was 0.8 ng/mL.At 2,20,80 ng/mL,the extraction efficiency of the blood and urine were 80.1%—110.3%and 87.9%—109.1%respectively and the RSD was less than 10%.This method can be applied to the qualitative and quantitative analysis of modafinil in blood and urine in cases.