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[Simultaneous determination of five hypertoxic rodenticides in serum by gas chromatography-mass spectrometry].

Se pu = Chinese journal of chromatography (2015-07-18)
Huiqiu Huang, Xun Huang, Jingsun Yu
ABSTRACT

A fast analytical method based on gas chromatography-mass spectrometry (GC-MS) was established for the simultaneous determination of tetramine, fluoroacetamide, sodium fluoroacetate, gliftor I and gliftor II in serum. At pH 2.0, sodium fluoroacetate was derivatizated at room temperature for 5 min by using N,N-diethyl-p-phenylenediamine as the derivatization reagent and N, N'-dicyclohexylcarbodiimide as the catalyst. The derivative and other rodenticides were extracted with ethyl acetate and concentrated with nitrogen at 50 °C, then determined by GC-MS in selected ion monitoring (SIM) mode, and quantified with matrix-match standard solutions. The analysis was carried out on an ionic liquid chromatographic capillary column (SLB-IL59, 30 m x 0.25 mm x 0.20 µm, maximum temperature 300 °C) at a flow rate of 1.0 mL/min, and the five rodenticides were successfully separated in 15 min when temperature programming was used. The results showed that the calibration curves were linear in the range of 0.01-1.0 mg/L, except for fluoroacetamide (0.02-2.0 mg/L) and tetramine (0.02-10 mg/L), with correlation coefficients (R2) greater than 0.995, and the limits of detection (LODs) were 0.001-0.002 mg/L (S/N = 3). The recoveries were 84.0%-110.0% at three different spiked levels, and the relative standard deviations (RSDs) were 2.9%-7.5% (n = 6). The method is simple, accurate, highly sensitive and suitable for the detection of the five hypertoxic rodenticides in serum for toxicological purposes.

MATERIALS
Product Number
Brand
Product Description

Supelco
SLB®-1ms Capillary GC Column, L × I.D. 30 m × 0.32 mm, df 0.10 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 60 m × 0.32 mm, df 0.25 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 30 m × 0.32 mm, df 0.25 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 20 m × 0.18 mm, df 0.18 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 0.10 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 60 m × 0.25 mm, df 0.25 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 0.25 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 15 m × 0.25 mm, df 0.25 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 15 m × 0.32 mm, df 0.25 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 10 m × 0.10 mm, df 0.40 μm
Supelco
SLB®-1ms Capillary GC Column, L × I.D. 10 m × 0.10 mm, df 0.10 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 1.00 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 15 m × 0.25 mm, df 0.25 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 0.50 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 30 m × 0.32 mm, df 0.25 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 30 m × 0.32 mm, df 0.50 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 30 m × 0.53 mm, df 1.00 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 10 m × 0.10 mm, df 0.10 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 15 m × 0.10 mm, df 0.10 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 20 m × 0.18 mm, df 0.18 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 0.25 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 60 m × 0.25 mm, df 0.25 μm
Supelco
SLB®-5ms Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 0.10 μm