羊毛脂中游离羊毛醇和残留农药的含量测定

Determination of Free Lanolin Alcohol and Residual Pesticides in Lanolin

关键词:  凝胶渗透色谱  气相色谱  羊毛脂  羊毛醇  残留农药

Key words:  gel permeation chromatography  gas chromatography  lanolin  lanolin alcohol  residual pesticides

摘要:

目的 采用气相色谱法测定羊毛脂中游离羊毛醇以及残留农药的含量，并评价方法可能性。方法 使用凝胶渗透色谱(gel permeation chromatography，GPC)进行前处理，分别采用气相色谱-火焰离子化检测器法(GC-FID)与气相色谱-质谱联用法(GC-MS)测定游离羊毛醇及残留农药的含量，以保留时间定性，总峰面积定量。结果 GPC前处理系统的回收率均符合要求。在建立的2种方法下，各待测物分离良好；线性关系良好(相关系数均>0.999 5)；平均回收率为90.49%~102.78%(n=6)。3个批次的羊毛脂中游离羊毛醇含量均<2.84%，另外1个批次的羊毛脂中有顺氯菊酯和反氯菊酯检出，其他残留农药均未检出。结论 本实验建立的GPC-GC/FID和GPC-GC/MS法专属性良好，精密度、准确度较高，耐用性好，可用于羊毛脂中游离羊毛醇和6种有机磷和拟除虫菊酯类残留农药的含量测定。同时，本研究可为羊毛脂质量控制提供参考。

Abstract:

OBJECTIVE To determine the content of free lanolin alcohol and residual pesticides in lanolin by gas chromatography, and to evaluate the feasibility of the established method. METHODS Gel permeation chromatography(GPC) was used for pretreatment, and the contents of free lanolin alcohol and residual pesticides were determined by GC-FID and GC-MS, respectively. And the qualitative analysis was conducted based on the retention time and quantitative analysis was conducted by total peak area. RESULTS The recovery of GPC pretreatment system met the requirements. Under the two established methods, the determinand were well separated; the satisfactory linearity with good correlation coefficients >0.999 5 were obtained; and the average recoveries were in the range of 90.49%-102.78%(n=6). The content of free lanolin alcohol in 3 batches of lanolin was <2.84%, cis-permethrin and trans-permethrin were determined in lanolin and the other residual pesticides were not detected. CONCLUSION The GPC-GC/FID and GPC-GC/MS method established in the study have good specificity, high precision, accuracy and robustness, which can be used for the separation and determination of free lanolin alcohol and six organophosphorus and pyrethroid residual pesticides in lanolin. At the same time, this study can provide reference for the quality control of lanolin.