氟硅唑和宁南霉素在橙汁加工过程中的残留动态与膳食风险评估  

Residue Dynamics and Dietary Risk Assessment of Flusilazole and Ningnanmycin in Citrus Juice Processing

作　　者：熊欢 何悦 刘磊 赵其阳[1,2,3] 张耀海 焦必宁[1,2,3] 王成秋 XIONG Huan;HE Yue;LIU Lei;ZHAO Qiyang;ZHANG Yaohai;JIAO Bining;WANG Chengqiu(Citrus Research Institute,Southwest University,Chongqing 400712,China;Laboratory of Quality and Safety Risk Assessment for Citrus Products,Ministry of Agriculture and Rural Affairs,Chongqing 400712,China;Quality Supervision and Testing Center for Citrus and Seedling,Ministry of Agriculture and Rural Affairs,Chongqing 400712,China)

机构地区：[1]西南大学柑桔研究所,重庆400712 [2]农业农村部柑桔产品质量安全风险评估实验室,重庆400712 [3]农业农村部柑桔及苗木质量监督检验测试中心,重庆400712

出　　处：《食品科学》2024年第14期249-256,共8页Food Science

基　　金：现代农业产业技术体系建设专项(CARS-26);柑橘类水果质量安全保障技术应用及示范项目(2019YFC1605604)。

摘　　要：目的:为明确氟硅唑和宁南霉素在柑橘及其加工制品中的安全性,在重庆、湖南两地进行田间实验,并按照橙汁商业化加工工艺进行加工,得到橙汁加工过程中氟硅唑和宁南霉素的残留动态及加工因子,并进行膳食风险评估。方法:分别采用QuEChERS(quick,easy,cheap,effective,rugged,and safe)方法和固相萃取法结合超高效液相色谱-串联质谱联用技术建立氟硅唑和宁南霉素在柑橘及其加工产品中的定量分析方法。结果:建立的方法准确度和灵敏度良好。在0.01、0.1、0.2 mg/kg(皮精油基质为0.05、0.5、2、20 mg/kg)加标水平下氟硅唑平均回收率为78.5%~108.4%,相对标准偏差(relative standard deviation,RSD)为0.5%~6.6%。在0.05、0.5、5 mg/kg(皮精油基质为0.05、0.5、5、20 mg/kg)加标水平下,宁南霉素平均回收率为88.3%~105.6%,RSD为0.3%~8.7%。在橙汁加工过程中,榨汁过程是降低氟硅唑和宁南霉素残留的高效途径,初榨果汁中两种农药残留量降低了93.3%~98.6%。皮渣中氟硅唑和宁南霉素易发生富集,精油中宁南霉素残留量降低而氟硅唑发生富集,其余加工产品中加工因子均小于1。氟硅唑和宁南霉素对不同年龄段人群的急性和慢性膳食暴露风险均低于100%,无不可接受风险。结论:本研究可为监测氟硅唑和宁南霉素在柑橘及其产品中的残留行为及膳食暴露风险评估提供参考,助推两种农药在柑橘生产中防病的科学应用。Objective:To assess the safety of flusilazole and ningnanmycin in citrus and its processed products,field trials were conducted in Chongqing and Hunan and orange juice processing was performed following the commercial procedure.The residue dynamics,processing factors and dietary nisk assessment of fusilazole and ningnanmycin during orange juice processing were investigated.Methods:The quick,easy,cheap,effective,rugged,and safe(QuEChERS)procedure and solid phase extraction(SPE)were employed to develop a quantitative analytical method for flusilazole and ningnanmypin in orange and its processed products using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),respectively.Results:The sensitivity and acuracy of the established method were good.In orange peel essential oil at 0.05,0.5,2 and 20 mg/kg,the average recoveries of fusilazole were 78.5%-1084%with relative standard deviation(RSD)between 0.5%and 6.6%at spiked levels of 0.01,0.1 and 0.2 mg/kg.In orange peel essential oil at 0.05,0.5,5 and 20 mg/kg,the average recoveries of ningnanmycin were 883%~-105.6%with RSD between 0.3%and 8.7%at spiked levels of 0.05,0.5 and 5 mg/kg.The squeezing process was a highly effective way to reduce the residues of flusilazole and ningnanmycin,which were reduced by 93.3%to 98.6%in mother juice,respectively.Both compounds were prone to enrichment in orange pomace.The residue level of ningnanmycin in the peel essential oil was reduced while that of flusilazole was enriched.Processing factors less than 1 were observed for the other processed products.The risks of acute and chronic dietary exposure to flusilazole and ningnanmycin among different age groups were both lower than 100%,which were at an acceptable 1evel.Conclusion:This study could provide a reference for residue behavior and dietary exposue risk assessment of fusilazole and ningnanmycin in citrus and its products,thereby promoting the scientific application of the two pesticides for disease prevention in the citrus indutry.

关 键 词：氟硅唑 宁南霉素 柑橘汁加工 农药残留 加工因子 

分 类 号：TS201.6[轻工技术与工程—食品科学]