title: Quantitative analysis of monofluoroacetate in biological samples by high-performance liquid chromatography using fluorescence labeling with 9-chloromethylanthracene.
abstract: A rapid and sensitive RP-HPLC method with fluorescence detection has been developed for the quantitative analysis of trace amounts of monofluoroacetate (MFA) in biological samples as serum, food and meat. 9-Chloromethylanthracene (9-CMA) is used as the fluorescence labeling reagent. Samples were extracted and reacted with 9-chloromethylanthracene together with tetrabutylammonium bromide as catalyst at 80 degrees C for 50 min to give a new fluorescent derivative as 9-methyleneanthracene monofluoroacetate (MA-MFA). The resulting MA-MFA was characterized with IR, (1)H NMR, (13)C NMR and MS. Chromatography separation is performed on an Agilent Hypersil ODS column with a fluorescent detector employed with the excitation and emission wavelengths as 256 nm and 412 nm, respectively. Optimal conditions for derivatization, fluorescence detection and chromatographic separation have been established. The novel method yields a good linear relationship when the MFA concentration in serum within 1 and 250 ng/mL (r=0.9988). The detection limit (signal-to-noise ratio=3 with 2 microL injected) was 0.25 ng/mL. The practical applicability of this method was demonstrated by quantitative determination of MFA-Na in a blood sample from a person who had ingested the poison.
authors: School of Chemistry and Chemical Engineering, Sun Yet-Sen University, Guangzhou, PR China.
authors: Zhenming
authors: Z
authors: Xie
authors: Wenbing
authors: W
authors: Shi
authors: Lan
authors: L
authors: Liu
authors: Qinying
authors: Q
authors: Deng
mesh_terms: D000818:Animals; D000873:Anthracenes / Q000032:analysis / Q000737:chemistry*; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D005240:Feasibility Studies; D005456:Fluorescent Dyes / Q000032:analysis / Q000737:chemistry*; D005463:Fluoroacetates / Q000032:analysis* / Q000097:blood / Q000737:chemistry / Q000506:poisoning; D005506:Food Contamination / Q000032:analysis*; D006801:Humans; D008460:Meat / Q000032:analysis* / Q000506:poisoning; D012275:Oryza / Q000737:chemistry* / Q000506:poisoning; D011041:Poisoning / Q000097:blood / Q000175:diagnosis; D000644:Quaternary Ammonium Compounds / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D044967:Serum / Q000737:chemistry; D013048:Specimen Handling; D013050:Spectrometry, Fluorescence; D013056:Spectrophotometry, Ultraviolet; D013552:Swine; D013696:Temperature
chemical_list: D000873:Anthracenes; D005456:Fluorescent Dyes; D005463:Fluoroacetates; D000644:Quaternary Ammonium Compounds; C099162:9-chloromethylanthracene; C014815:fluoroacetic acid; C009405:tetrabutylammonium