GC-MS法快速检验食材及呕吐物中的氟乙酸钠

GC-MS Rapidly Determining Sodium Fluoroacetate in Samples of Food Poisoning

目的 开发一种新方法,对中毒案件食物检材及呕吐物中的氟乙酸(盐)进行快速气相色谱-质谱(GC-MS)检验。方法 体外检材经纯水提取后,在水相中添加含衍生化试剂五氟苄基溴(PFB-Br)的有机溶剂,在相转移催化剂四丁基硫酸氢铵(IPC-TBA-HS)的作用下实现同步衍生提取分离;使用配备有HP-5MS弹性石英毛细管柱(30m×0.25mm×0.25mm)的GC-MS进行分析;以衍生化产物氟乙酸五氟苄基酯(PFB-MFA)的保留时间和特征碎片离子m/z 181.0(定量离子)、258.0、61.0及特征峰面积作为定性、定量的依据。结果该方法在0.1~10μg/mL的浓度范围内呈良好线性关系(R^(2)=0.9997, n=7),检出限为0.050μg/mL,方法回收率大于80%。结论 经验证,所开发的方法省时省力、简便易于操作、灵敏度高,适用于基层一线检验部门。

Objective To develop a new derivatization method for GC-MS to rapidly determine fl uoroacetate(salt) from food-poisoning samples and vomit. Methods The samples were extracted with pure water, then added of the organic solvent containing derivatization reagent(PFB-Br) into the aqueous phase so that the derivatization-synchronous extraction was achieved under the function of tetrabutylammonium hydrogen sulfate(also named as IPC-TBA-HS), a phase transfer catalyst(PTC). GC-MS, equipped with HP-5MS elastic quartz capillary column(30m×0.25mm×0.25mm), was adopted for analysis into the extractant. From the retention time of pentafl uorobenzylmono-fl uoroacetate(PFB-MFA)(the derivatized product),the relevant fragmented ions of m/z 181.0, 258.0, 61.0 and involving characteristic peak areas were selected as qualitative and quantitative benchmark. Results The method was showing linear among 0.1μg-10μg/ml(R^(2)=0.9997, n=7), with its detection limit as 0.050ug/ml and recovery being more than 80%. Conclusions The developed method has been verifi ed of time-saving,less workload, simplicity, easiness to operate and high sensitivity, suitable for frontline detection units to utilize, too.