固相萃取/液相色谱-串联质谱法测定沃柑春雷霉素和双胍辛胺残留  

Determination of residues of kasugamycin and iminoctadine in Orah mandarin using Solid-Phase Extraction/HPLC-MS/MS method

作　　者：何京明 苏丽梅 石梁稳 唐标 韦东 李治尧 黄梅贵 刘守廷 班燕宁 HE Jingming;SU Limei;SHI Liangwen;TANG Biao;WEI Dong;LI Zhiyao;HUANG Meigui;LIU Shouting;BAN Yanning(Guangxi Boce Test Technical Services Co.Ltd.,Nanning,Guangxi,530007,China;Guangxi Zhuang Autonomous Region Quality Test Research Institute of Product Quality,Nanning,Guangxi,530007,China;Guangxi Zhongsheng Biotechnology Co.Ltd.,Nanning,Guangxi,530105,China;Nanning Wuming District Cash Crop Technical Service Center,Nanning,Guangxi,530199,China)

机构地区：[1]广西博测检测技术服务有限公司,南宁530007 [2]广西壮族自治区产品质量检验研究院,南宁530007 [3]广西众晟生物科技有限公司,南宁530105 [4]南宁市武鸣区经济作物技术服务中心,南宁530199

出　　处：《中国南方果树》2024年第5期43-52,共10页South China Fruits

基　　金：广西壮族自治区南宁市重点研发项目(20212149);广西壮族自治区重点研发项目(桂科AB23075085)资助。

摘　　要：春雷霉素和双胍三辛烷基苯磺酸盐是沃柑生产中常用的杀菌剂。为了建立采用固相萃取/高效液相色谱-质谱联用技术(HPLC-MS/MS)同时提取同步测定春雷霉素和双胍三辛烷基苯磺酸盐在沃柑果实中残留的方法,开展了提取剂筛选、提取液净化方法筛选、液相色谱流动相体系筛选试验,并对方法的重复性和再现性进行了验证。结果表明,沃柑果实匀浆样品用0.2%(体积分数)甲酸水溶液提取后,先采用HLB固相萃取柱净化,再分别经SCX固相萃取柱、WCX固相萃取柱除去干扰物质,然后用C18-AQ高效液相色谱柱在正电喷雾模式下进行多重反应监测(MRM)分析,以沃柑空白基质匹配标准工作溶液进行外标法定量,可实现准确的定性分析和精确的定量分析。在0.005~0.500 mg/L范围内,春雷霉素和双胍辛胺浓度与峰面积呈良好的线性关系,线性相关系数分别为0.9999和0.9995。方法的灵敏度高,对沃柑中春雷霉素和双胍辛胺的检出限为0.001 mg/kg,定量限为0.004 mg/kg,对春雷霉素和双胍辛胺的加标(500~8000 ng/10 g试样)回收率分别为64.48%~98.42%和62.38%~85.86%。方法的再现性好,不同检测机构间春雷霉素和双胍辛胺检测结果的相对标准偏差分别为9.89%和9.75%。Kasugamycin and iminoctadine tris are commonly used fungicides in Orah production.To set up a method for the simultaneous extraction and determination of kasugamycin and iminoctadine tris residues in Orah fruits using Solid-Phase Extraction(SPE)and High-Performance Liquid Chromatography-Tandem Mass Spectrometry(HPLC-MS/MS),the screening test of extraction agent,the extract purification method,and the liquid chromatography mobile phase system was conducted,and the repeatability and reproducibility of the method were verified.The results showed that the samples were extracted with a 0.2% formic acid aqueous solution,purified with HLB SPE columns,and then interfering substances were removed using strong cation-exchange(SCX)and weak cation-exchange(WCX)SPE columns,respectively.The analysis was performed on a C18-AQ HPLC column in positive electrospray ionization mode with Multiple Reaction Monitoring(MRM).Quantification was conducted using an external standard calibration curve with blank matrix-matched standards,the residues of kasugamycin and iminoctadine can be qualitatively and quantitatively analyzed accurately.There was a good linear relationship between the concentration and peak area of kasugamycin and iminoctadine within the concentration range of 0.005 to 0.500 mg/L,with linear correlation coefficients of 0.9999 and 0.9995,respectively.The method demonstrated high sensitivity,with limits of detection(LOD)of 0.001 mg/kg and limits of quantification(LOQ)of 0.004 mg/kg for both kasugamycin and iminoctadine in Orah.The spiking recoveries ranged from 64.48% to 98.42% for kasugamycin and from 62.38%to 85.86%for iminoctadine.The method showed good repeatability,with relative standard deviations(RSD)of 9.89% and 9.75% for Kasugamycin and Iminoctadine,respectively,across different laboratories.

关 键 词：沃柑 液相色谱-质谱 春雷霉素 双胍辛胺 

分 类 号：S481.8[农业科学—农药学]