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Development and validation of carbofuran and 3-hydroxycarbofuran analysis by high-pressure liquid chromatography with diode array detector (HPLC-DAD) for forensic Veterinary Medicine
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2017-09-14 , DOI: 10.1016/j.jchromb.2017.09.021
Vagner Gonçalves , Nicolle Queiroz Hazarbassanov , Adriana de Siqueira , Jorge Camilo Florio , Claudia Helena Pastor Ciscato , Paulo Cesar Maiorka , André Rinaldi Fukushima , Helenice de Souza Spinosa

Agricultural pesticides used with the criminal intent to intoxicate domestic and wild animals are a serious concern in Veterinary Medicine. In order to identify the pesticide carbofuran and its metabolite 3- hydroxycarbofuran in animals suspected of exogenous intoxication a high pressure liquid chromatography with diode array detector (HPLC-DAD) method was developed and validated in stomach contents, liver, vitreous humor and blood. The method was evaluated using biological samples from seven different animal species. The following parameters of analytical validation were evaluated: linearity, precision, accuracy, selectivity, recovery and matrix effect. The method was linear at the range of 6.25–100 μg/mL and the correlation coefficient (r2) values were >0.9811 for all matrices. The precision and accuracy of the method was determined by coefficient of variation (CV) and the relative standard deviation error (RSE), and both were less than 15%. Recovery ranged from 74.29 to 100.1% for carbofuran and from 64.72 to 100.61% for 3-hydroxycarbofuran. There were no significant interfering peaks or matrix effects. This method was suitable for detecting 25 positive cases for carbofuran amongst a total of 64 animal samples suspected of poisoning brought to the Toxicology Diagnostic Laboratory, School of Veterinary Medicine and Animal Sciences, University of Sao Paulo.



中文翻译:

高压液相色谱法与二极管阵列检测器(HPLC-DAD)结合用于法医兽医学中的呋喃呋喃和3-羟基呋喃呋喃分析的开发和验证

在兽医学中,出于令人陶醉的目的而使用的农业农药会引起家畜和野生动物的醉酒。为了在怀疑有外源性中毒的动物中鉴定农药呋喃丹及其代谢物3-羟基碳呋喃,开发了带有二极管阵列检测器(HPLC-DAD)方法的高压液相色谱法,并在胃内容物,肝脏,玻璃体液和血液中进行了验证。使用来自七个不同动物物种的生物样品评估了该方法。评估了以下分析验证参数:线性,精密度,准确性,选择性,回收率和基质效应。该方法在6.25–100μg/ mL范围内呈线性,相关系数为(r 2)所有矩阵的值均> 0.9811。该方法的精密度和准确性由变异系数(CV)和相对标准偏差误差(RSE)决定,二者均小于15%。呋喃喃的回收率范围从74.29%到100.1%,3-羟基呋喃呋喃的回收率从64.72%到100.61%。没有明显的干扰峰或基质效应。该方法适用于从圣保罗大学兽医与动物科学学院毒理学诊断实验室收集的总共64份怀疑中毒的动物样本中,检测25例呋喃丹的阳性病例。

更新日期:2017-09-14
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