摘要
建立了以4-溴甲基7-甲氧基香豆素(BrMMC)为柱前荧光衍生试剂,反相高效液相色谱荧光检测(HPLC-FLD)生物检材中氟乙酸钠的分析方法。采用Hewlett Packard RP-18色谱柱,以甲醇-水(60/40,V/V)为流动相,流速1.0mL/min,柱温26℃,荧光检测:λex=319nm,λem=390nm,进样量2μL。结果表明:该法在氟乙酸钠含量为0.1~20μg/mL范围内与其峰面积呈良好的线性关系,线性相关系数为0.9996,检出限(S/N=3)为5×10^-10mol/mL,相对标准偏差(RSD)小于4%。本法用于中毒死亡者的血液样品及其它检材的测定,效果良好。
A method was developed for the determination of trace amounts sodium monofluoroacetate (MFA-Na, 1080) in biological samples by high-performance liquid chromatography (HPLC) with fluorescence detector (FLD). The use of 4-bromomethyl-7-methoxycoumarin (BrMMC) as a fluorescencelabeling reagent has been investigated. The HPLC with a Hewlett Packard RP-18 column and the fluorescence detector at λex 319nm/λem 390nm was employed using 1 mL/min methanol-water (60/40, V/V) as mobile phase. The calibration curve of MFA-Na had a linear range of 0. 1-20μg/mL with r=0. 999 6 and a detection limit of 5×10^-10 mol/mL (S/ N=3). The relative standard deviation (RSD) was less than 4%. The practical applicability of the method to biological samples was demonstrated by samples of water and serum that were spiked with MFA-Na and by a sample of an individual with MFA-Na consumption.
出处
《分析科学学报》
CAS
CSCD
2007年第6期685-688,共4页
Journal of Analytical Science
基金
广东省科技计划资助项目(No.2001C32202)
广东省公安厅科研基金资助项目(2001)