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 fluoroacetate,gliftor Ⅰand gliftor Ⅱ in serum. At pH 2. 0,sodium fluoroacetate was derivatizated at room temperature for 5min 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 of0. 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.
出处
《色谱》
CAS
CSCD
北大核心
2015年第3期323-328,共6页
Chinese Journal of Chromatography
关键词
气相色谱-质谱
剧毒灭鼠剂
血清
gas chromatography-mass spectrometry（GC-MS）
hypertoxic rodenticide
serum
作者简介
通讯联系人．Tel：（0577）63038031，E-mail：hhqq2002@sina．com．
