ABSTRACT
OBJECTIVE: To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS) method for simultaneous detection of 12 kinds of rodenticides such as tetramine, warfarin and rodenticide in suspected poisoning patients' residual food, vomit, gastric lavage, serum and urine. METHODS: The residual food, vomit, gastric lavage, serum and urine of patients with suspected rodenticide poisoning were collected. The food, vomit, gastric lavage and urine samples were added with ammonium acetate at a concentration of 2 mol/L, and than were repeatedly extracted twice by ethyl acetate. The serum sample was extracted by adding acetonitrile. After the sample was dried by nitrogen, it was dissolved in methanol ∶ammonium acetate(60 ∶40, V/V), and the supernatant was centrifuged and separated by a C18 column, and quantified by a standard curve method. Samples were detected by HPLC-MS. RESULTS: The linearity of the 12 kinds of rodenticides in the quantitative range of residual food, vomit, gastric lavage, serum and urine in patients with suspected rodenticide poisoning was good, and the correlation coefficient was 0.992 3-0.999 9. The detection limit of food, vomit or gastric lavage was 0.03-0.14 μg/kg, and that in serum and urine were 0.10-0.30 and 0.02-0.04 μg/L, respectively. The standard recovery rate was 84.4%-114.0%, and the within-run and between-run relative standard deviations were 2.7%-6.2% and 2.4%-9.5%, respectively.CONCLUSION: The method has advantages of simple operation, high efficiency and good accuracy. This method is suitable for emergency treatment of poisoning events caused by rodent drugs or poisoning.
ABSTRACT
A sensitive method was developed for the determination of pacific ciguatoxin (P-CTX1) residue in fishes by high performance liquid chromatography coupled with electrospray tandem mass spectrometry ( HPLC-MS/MS). Homogenized samples of fish was extracted with acetone,degreased by freezing under -20℃ and filtered with filter paper. Then the supernatant was cleaned up with PSA column. Identification was achieved by electrospray ionization (ESI) in positive mode using multiple reaction monitoring. The calibration curve of P-CTX1 showed good linearity in the range of 0.5 -20μg/L with correlation coefficient of 0.9998. The limit of quantitation (LOQ) was 0. 1 mg/L( S/N = 10). The recoveries of P-CTX1 were between 82. 3% and 87. 2% (n =7) at spiked levels of 1.0 -20.0 ng/kg. The relative standard derivations( RSD) of the method were less than 7.8%.