基于超声辅助-液相色谱法的大米中氟环唑残留检测  

Detection of epoxiconazole residue in the rice by ultrasound-assisted liquid chromatography

作　　者：张达 陈柯宏 ZHANG Da;CHEN Ke-hong(Hongji Testing Technology Center Co.,Ltd.,Ningbo 315000,China;Ningbo Guoqing Testing Technology Co.,Ltd.,Ningbo 315303,China)

机构地区：[1]宁波市中技检测技术中心有限公司,浙江宁波315000 [2]宁波国清检测技术有限公司,浙江宁波315303

出　　处：《粮食与饲料工业》2024年第4期67-69,76,共4页Cereal & Feed Industry

摘　　要：通过超声辅助-液相色谱法快速检测大米中的氟环唑残留。试验首先对样品前处理条件进行优化,然后对方法重复性和加标回收率进行测试。试验结果表明,提取剂为丙酮,固液比(样品与丙酮比例)为1∶9,氯化钠用量为3 g,超声提取时间为8 min的条件下,对大米样品中的氟环唑提取效果最好。在0.01~1.2μg/mL的浓度范围内,氟环唑的质量浓度与色谱峰面积线性相关系数R 2=0.99,最低检测限为0.01 mg/mL,重复性实验的相对标准偏差RSD为1.77%,加标回收率范围为89.0%~90.1%。超声辅助-液相色谱法可以快速萃取大米样品中的氟环唑,提高萃取效果,节约实验时间,对大米中的氟环唑进行有效测定。This study aims to rapidly detect the epoxiconazole residue in the rice by using ultrasound-assisted liquid chromatography.In the test,we optimized the sample pretreatment conditions first and then tested on methodological repeatability and standard addition recovery rate.The results indicate the epoxiconazole residue in the rice is best extracted when extractant is acetone,solid-to-liquid ratio(or sample to acetone ratio)is 1∶9,sodium chloride dosage is 3 g,and ultrasound extraction lasts 8 min.In 0.01-1.2μg/mL concentration range,the linear correlation coefficient of epoxiconazole mass concentration and chromatographic peak area R 2 is 0.99,the minimum limit of detection is 0.01 mg/mL,the relative standard deviation(RSD)of repeat tests is 1.77%,and the standard addition recovery rate range is 89.0%-90.1%.It is made clear through the trial that the ultrasound and chromatography could speed up detection of epoxiconazole residue in the rice,improve extraction effect,save the test time,and accomplish an effective determination of epoxiconazole in the rice.

关 键 词：大米 氟环唑残留 检测分析 食品安全 超声辅助萃取 液相色谱 

分 类 号：TS201.6[轻工技术与工程—食品科学]