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建立了同时快速测定血清样品中毒鼠强、氟乙酰胺、氟乙酸钠、甘氟Ⅰ与甘氟Ⅱ5种灭鼠剂的气相色谱-质谱联用法。在 pH 2.0条件下,以 N,N-二乙基对苯二胺为衍生剂,N,N′-二环己基碳二亚胺为催化剂,氟乙酸钠在室温下振荡衍生5 min,衍生物与毒鼠强、氟乙酰胺、甘氟Ⅰ、甘氟Ⅱ一并被乙酸乙酯萃取,经50℃下氮吹浓缩后用气相色谱-质谱同时测定,采用选择离子监测( SIM)模式,基质标准外标法定量。方法选用 SLB-IL59离子液体毛细管柱(30 m×0.25 mm×0.20μm,最高温度:300℃),流速1.0 mL/min,经程序升温在15 min内成功地分离了5种灭鼠剂。结果显示,血清中氟乙酰胺的线性范围为0.02~2.0 mg/L,毒鼠强的线性范围为0.02~10 mg/L,其他目标物的线性范围为0.01~1.0 mg/L;检出限为0.001~0.002 mg/L( S/N=3),相关系数 R2>0.995。在3个加标水平下,方法加标回收率介于84.0%和110.0%之间,相对标准偏差( n=6)介于2.9%和7.5%之间。方法操作简便、准确,灵敏度高,适于中毒病人的快速诊断检测。

A fast analytical method based on gas chromatography-mass spectrometry( GC-MS) was established for the simultaneous determination of tetramine,fluoroacetamide,sodium flu-oroacetate,gliftorⅠ and gliftorⅡ 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 rodenti-cides were extracted with ethyl acetate and concentrated with nitrogen at 50 ℃,then deter-mined 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×0. 25 mm×0. 20 μm,maximum temperature 300 ℃)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 dif-ferent 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.

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