用高效液相色谱法定量分析氰烯菌酯

超高效液相色谱-串联质谱法测定食品中烯肟菌酯残留量吴洁珊;陈亮;冯家望;任永霞;蔡勤仁【摘要】UHPLC-MS/MS was applied to determination of residual amount of enostrobilurin in food.The sample was extracted with acetonitrile and purified by dispersive solid phase extraction with primary secondary amine,C18 and anhydrous MgSO4 as extractants.The eluate obtained were used for UHPLC-MS/MS determination,in which Eclipse Plus C18 column (50 mm× 2.1 mm,1.8 μm)was used as stationary phase,and a mixture of acetonitrile and 5 mmol · L-1 ammonium acetate (75 +25) was used as mobile phase; positive electrospray ionization was used in the detection.Linear relationship between values of peak area and mass concentration of enostrobilurin was kept in the range within 50 μg · L-1,with detection limit (3S/N) of 1 μg·kg-1.On the base of blank sample,test for recovery was made by standard addition method; values of average recovery found were in the range of 76.7％-89.6％,with RSD's (n=10) in the range of 4.2％-11％.%提出了用超高效液相色谱-串联质谱法测定食品中烯肟菌酯残留量的方法.样品经乙腈提取后,以伯仲胺、C18和无水硫酸镁为萃取剂用基质分散固相萃取净化,净化液经Eclipse PlusC18色谱柱(50 mm×2.1mm,1.8μm)分离,用乙腈与5 mmol·L-1乙酸铵溶液(75+25)的混合液洗脱,采用正离子模式监测.烯肟菌酯的质量浓度在50μg·L-1以内与峰面积呈线性关系,检出限(3S/N)为1μg·kg-1,以空白样品为基体进行加标回收试验,所得回收率在76.7％～89.6％之间,相对标准偏差(n=10)在4.2％～11％之间.【期刊名称】《理化检验-化学分册》【年(卷),期】2013(049)008【总页数】4页(P953-956)【关键词】超高效液相色谱-串联质谱法;烯肟菌酯;食品【作者】吴洁珊;陈亮;冯家望;任永霞;蔡勤仁【作者单位】珠海出入境检验检疫局,珠海519015;珠海出入境检验检疫局,珠海519015;珠海出入境检验检疫局,珠海519015;珠海出入境检验检疫局,珠海519015;珠海出入境检验检疫局,珠海519015【正文语种】中文【中图分类】O657.63烯肟菌酯是一种新型广谱的甲氧基丙烯酸酯杀菌剂，为国内开发的第一个甲氧基丙烯酸酯类杀菌剂，具有杀菌谱广、活性高、毒性低，与环境相容性好等特点，并已大面积推广应用于水稻、小麦、黄瓜、番茄和马铃薯等作物中［1－2］。

高效液相色谱法分析氰戊菊酯微乳剂、水乳剂丁轶聪;李琦;孙伟嘉【期刊名称】《化学分析计量》【年(卷),期】2015(0)1【摘要】采用异丙醇提取微乳剂型和水乳剂型氰戊菊酯样品中的有效成分氰戊菊酯，以正相高效液相色谱法测定氰戊菊酯含量。

样品提取后用流动相定容，经0.45µm针式有机滤膜过滤，通过lnertsil SIL–100A硅胶色谱柱进行分离，以正己烷–乙酸乙酯（体积98∶2）作为流动相，流量为2 mL／min，紫外检测波长为254 nm，柱温为30℃，外标法定量。

氰戊菊酯的质量浓度在0.8～4.0 mg／mL 范围内与色谱峰面积呈良好的线性关系，相关系数r=0.9996，检出限为10µg／mL。

在3个添加水平下，样品的加标回收率在89.2%～98.6%之间，测定结果的相对标准偏差均小于3%(n=6)。

该方法快速、简单、准确，可用于批量样品的氰戊菊酯成分定量定性检验。

%Isopropyl alcohol was used to extract the active ingredient fenvalerate in water emulsions and microemul-sion fenvalerate sample, fenvalerate content was determined by normal phase high performance liquid chromatography. After being extracted, the sample solution was mixed with mobile phase, filted with organic needle 0.45μm membrane filter, then separated by silica gel column. Hexane–ethyl acetate (volume rate was 98∶2) was used as mobile phase with flow rate of 2mL/min, UV wavelength was at 254 nm,column temperature was30℃.External standard method was used. Fenvalerate concentration was linear with the chromatographic peak area in the range of 0.8–4.0 mg/mL,and the correlation coefficient r was 0.999 6,the detection limit was 10μg/mL. In the three spiked levels, recoveries were 89.2%–98.6%,and the relative standard deviation of detection results was less than 3%(n=6). The method is rapid,simple and accurate for fenvalerate quantitative and qualitative detection of the bulk sample.【总页数】3页(P77-79)【作者】丁轶聪;李琦;孙伟嘉【作者单位】阜阳市产品质量监督检验所，安徽阜阳 236000;阜阳市产品质量监督检验所，安徽阜阳 236000;阜阳市产品质量监督检验所，安徽阜阳 236000【正文语种】中文【中图分类】O657.7【相关文献】1.溶剂对S-氰戊菊酯微乳剂配方筛选的影响 [J], 朱恒营;路福绥;高翠丽;陈甜甜2.20%氰戊菊酯微乳剂的研制 [J], 仙鸣;刘哲峰;兀新养;谭涓3.8%氰戊菊酯微乳剂的研究 [J], 陈蔚林;吴秀华4.20%氰戊菊酯水乳剂防治菜青虫田间药效试验 [J], 黄雄英;周小毛5.5%S-氰戊菊酯微乳剂加工及性状简介 [J], 马洪艳;田学文;孙景文;王凤芝;李波;桂永珍因版权原因，仅展示原文概要，查看原文内容请购买。