摘要
建立了离子色谱-三重四极杆质谱测定血浆和尿液样品中氟乙酸(MFA)的方法。血浆样品经高氯酸超声提取,尿液样品经高氯酸酸化,血浆和尿液提取液在pH 0. 5~1. 0条件下用叔丁基甲醚(MTBE)萃取,萃取液经氮吹浓缩后溶于0. 1%(v/v)氨水溶液。以Ionpac AS 19型阴离子色谱柱为分析柱,在线自动产生的氢氧化钾作为淋洗液进行梯度分离,柱流出液经阴离子抑制器抑制后进入质谱系统。采用电喷雾电离源,在负离子、多离子监测(MRM)模式下检测,13C2-氟乙酸稳定同位素内标法定量。血浆和尿液样品中氟乙酸的平均加标回收率为96. 2%~120%,相对标准偏差为1. 1%~13. 1%(n=6),方法的检出限(S/N=3)分别为0. 03μg/L和0. 1μg/L。该法简单、灵敏、准确,可用于生物样品中氟乙酸的检测。
A method was developed for the determination of monofluoroacetic acid （MFA） in plasma and urine by ion chromatography-triple quadrupole mass spectrometry （IC-MS/MS）. A plasma sample was extracted with 3% （v/v） perchloric acid aqueous solution, and the extract was centrifuged to remove the protein and lipids. A urine sample was acidulated with 3% （v/v） perchloric acid aqueous solution. The target analyte was extracted with methyl tert-butyl ether （MTBE） at a pH between 0.5 and 1.0. After the MTBE was removed by blowing with nitrogen, the MFA in the residues was dissolved into 0.1% （v/v） ammonia solution. The separation of MFA was carried out on a Dionex Ionpac AS 19 analytical column （250 mm×2 mm, 7.5 μm） with gradient elution using KOH solution electrolytically generated from an on-line eluent generation cartridge. Before the eluent flow entered the mass spectrometer, an in-line suppressor was used to remove potassium ions. The MFA was detected with a negative electrospray ionization source in the multiple reaction monitoring （MRM） mode, and quantified with the stable isotope internal standard method. The correlation coefficient of the linear calibration curve of MFA was greater than 0.999 at the corresponding ranges of 0.1-1000 μg/L. The average recoveries were 96.2%-120% of MFA in plasma and urine samples with relative standard deviations of 1.1%-13.1% （n=6）. The limits of detection of MFA in plasma and urine samples were 0.03 μg/L and 0.1 μg/L, respectively. The method is simple, sensitive and accurate, and can be applied for the determination of MFA in plasma and urine samples.
作者
张晓艺
张秀尧
蔡欣欣
李瑞芬
ZHANG Xiaoyi;ZHANG Xiuyao;CAI Xinxin;LI Ruifen(Wenzhou Municipal Center for Disease Control and Prevention,Wenzhou 325001,China)
出处
《色谱》
CAS
CSCD
北大核心
2018年第10期979-984,共6页
Chinese Journal of Chromatography
关键词
离子色谱
三重四极杆质谱
氟乙酸
血浆
尿液
生物样品
ion chromatography （IC）
triple quadrupole mass spectrometry （MS/MS）
monofluoroacetic acid
plasma
urine
biological samples
