色谱

色谱 ›› 2015, Vol. 33 ›› Issue (3): 323-328.DOI: 10.3724/SP.J.1123.2014.11024

• 技术与应用 • 上一篇    

气相色谱-质谱法同时快速测定血清中5种剧毒灭鼠剂

黄会秋, 黄逊, 余惊笋   

  1. 平阳县疾病预防控制中心, 浙江 温州 325400
  • 收稿日期:2014-11-17 修回日期:2014-12-30 出版日期:2015-03-08 发布日期:2015-02-12
  • 通讯作者: 黄会秋

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

HUANG Huiqiu, HUANG Xun, YU Jingsun   

  1. Pingyang County Center For Disease Prevention and Control, Wenzhou 325400, China
  • Received:2014-11-17 Revised:2014-12-30 Online:2015-03-08 Published:2015-02-12

PDF

182

被引次数

7

摘要：

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Ⅱ 5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×0.20 μm,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。

关键词: 剧毒灭鼠剂, 气相色谱-质谱, 血清

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 ℃, 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×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 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.

Key words: gas chromatography-mass spectrometry (GC-MS), hypertoxic rodenticide, serum

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