Rapid identification and determination of the rodenticide valone in serum by high-performance liquid chromatography-tandem mass spectrometry.
Valone is a chronic anticoagulant rodenticide that has come into wide use in China. Current literature lacks analytical methods for the determination of valone. In this paper, a sensitive and selective assay was established for the identification and quantification of valone in serum by liquid chromatography-tandem mass spectrometry. After addition of the internal standard, warfarin, serum samples were extracted with 10% methanol in acetonitrile and cleaned using Oasis HLB solid-phase extraction (SPE) cartridges. The compounds were separated on an Agilent SB C18 column with a mobile phase of methanol/acetic acid-ammonium acetate (5 mmol/L, pH 6.3) (75:25, v/v). Detection was performed by electrospray ionization ion trap mass spectrometry in the negative multiple reaction monitoring mode. The transition ions of m/z 229 --> 145 and m/z 307 --> 161 were selected for quantification of valone and the internal standard, respectively. The overall extraction efficiency was between 81.1% and 91.1%. The limit of quantification was 0.5 ng/mL. Regression analysis of the calibration data revealed good correlation (r(2) > 0.99) for valone. Intra- and interday precisions for quality-control samples were less than 7.8% and 12.8%, respectively. This method combines a rapid SPE procedure with an extremely fast chromatographic analysis, which is especially advantageous or clinical laboratories.
Cai
Mei-Qiang
MQ
College of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310035, China.
Chen
Xiao-Hong
XH
Ouyang
Xiao-Kun
XK
Jin
Mi-Cong
MC
D000328:Adult; D000440:Butanols / Q000097:blood* / Q000506:poisoning; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005260:Female; D006801:Humans; D007192:Indenes / Q000097:blood* / Q000506:poisoning; D008297:Male; D011041:Poisoning / Q000097:blood; D012015:Reference Standards; D015203:Reproducibility of Results; D012378:Rodenticides / Q000097:blood* / Q000506:poisoning; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013997:Time Factors; D055815:Young Adult
D000440:Butanols; D007192:Indenes; D012378:Rodenticides; C540723:valone