Determination of Azoxystrobin Residue in Strawberries by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
摘 要
称取样品10.00 g,加入20.00 mL乙腈,高速匀浆2 min后,用滤纸过滤,滤液收集到装有5 g氯化钠的100 mL具塞量筒中,盖上塞子,剧烈振荡2 min,静置30 min。取上清液10.00 mL加入已经过5 mL乙腈-甲苯(3+1)混合液预淋洗的Carbon/NH2固相萃取小柱,收集淋洗液,用20 mL乙腈-甲苯(3+1)混合液分4次洗脱,合并淋洗液,于40℃水浴蒸发至近干,用甲醇(1+1)溶液定容至5.00 mL,旋涡混匀后,过0.22 μm滤膜。滤液经Waters XBridge C18色谱柱(3.0 mm×50 mm,3.5 μm)分离,以甲醇、乙腈和0.1%(体积分数)甲酸溶液为流动相进行梯度洗脱,质谱分析中采用电喷雾正离子源和多反应监测模式,以外标法定量。嘧菌酯质量浓度在0.001~0.10 mg·L-1与定量离子峰面积呈线性关系,检出限(3S/N)为0.10 μg·kg-1。方法用于测定草莓中的嘧菌酯残留,加标回收率为78.0%~95.2%,测定值的相对标准偏差(n=6)小于7.0%。
Abstract
The sample (10.00 g) was added into 20.00 mL of acetonitrile, and the mixture was homogenized for 2 min at a high speed, and filtered with a filter paper. The filtrate was collected into a 100 mL cylinder containing 5 g of sodium chloride, and the cylinder was covered with a stopper and shaked vigorously for 2 min. After standing for 30 min, 10.00 mL of the supernatant was taken and purified with a Carbon/NH2 solid phase extraction cartridge, which had been pre-rinsed with 5 mL of acetonitrile-toluene (3+1) mixture. The eluent was collected, and the cartridge was eluted with 20 mL of acetonitrile-toluene (3+1) mixture in 4 portions. The eluent was combined and evaporated to near dryness in a water bath at 40℃. The residue was made up to a volume of 5.00 mL with methanol (1+1) solution, and then the solution was vortexed well and then passed through a 0.22 μm filter membrane. The filtrate was separated on a Waters XBridge C18 column (3.0 mm×50 mm, 3.5 μm), with methanol, acetonitrile and 0.1% (volume fraction) formic acid as mobile phase for gradient elution. Electrospray positive ion source and multiple reaction monitoring mode were used for mass spectrometry analysis. External standard method was used for quantification. Linear relationship between values of the quantitative ion peak area and the mass concentration of azoxystrobin was obtained in the range of 0.001-0.10 mg·L-1, with the detection limit (3S/N) of 0.10 μg·kg-1. The proposed method was applied to determination of azoxystrobin residues in strawberries, giving values of recovery obtained by standard addition method in the range of 78.0%-95.2%, and RSDs (n=6) less than 7.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201812016
所属栏目 工作简报
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收稿日期 2017/11/2
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备注杜鑫,硕士,农艺师,主要研究方向为农产品质量安全检测分析,duxin2009@163.com
引用该论文: DU Xin,LI Guolie,SU Xu,QIN Mingli. Determination of Azoxystrobin Residue in Strawberries by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(12): 1445~1448
杜鑫,李国烈,苏旭,覃明丽. 超高效液相色谱-串联质谱法测定草莓中嘧菌酯的残留量[J]. 理化检验-化学分册, 2018, 54(12): 1445~1448
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【4】思彬彬,杨卓.甲氧基丙烯酸酯类杀菌剂作用机理研究进展[J].世界农药, 2007,29(6):5-9.
【5】伊海静,陈艳,刘正坪,等.草莓枯萎病菌的分离鉴定及防治药剂筛选[J].西北农业学报, 2016,25(4):626-635.
【6】朱卫刚,胡伟群,张蕊蕊,等.5种新型杀菌剂对草莓白粉病的生物活性研究[J].中国南方果树, 2014,43(3):114-115.
【7】杨振华,魏朝俊,贾临芳,等.SPE-GC法同时检测草莓中7种常用农药的残留[J].农业环境科学学报, 2012(11):2304-2308.
【8】黄海波.气相色谱法检测番茄果实中的嘧菌酯残留[J].南方农业, 2016,10(6):168-170.
【9】王亚慧,侯志广,密东林,等.高效液相色谱法同时测定马铃薯及其土壤中的霜脲氰和嘧菌酯[J].农药, 2014,53(11):815-817.
【10】石峰,赵科华,车军,等.高效液相色谱法分析砂糖桔中嘧菌酯残留[J].河北农业科学, 2010,14(2):161-163.
【11】高智席,江忠远,王柏人,等.水果和蔬菜中嘧菌酯的固相萃取-反相高效液相色谱测定法[J].环境与健康杂志, 2011,28(8):719-720.
【12】王军,代艳娜,黄利英,等.液相色谱-串联质谱法快速测定蔬菜中10种保鲜剂残留量[J].食品安全质量检测学报, 2015(6):2379-2385.
【13】林童,魏玉海,凤晓博,等.超高效液相色谱-串联质谱法测定枸杞中常见的5种农药残留[J].现代农药, 2015(1):37-39.
【14】吴岩,姜冰,徐义刚,等.QuEChERS-液相色谱-串联质谱法同时测定果蔬中16种农药残留[J].色谱, 2015,33(3):228-234.
【15】MATUSZEWSKI B K, CONSTANZER M L, CHAVEZENG C M. Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J]. Analytical Chemistry, 2003,75(13):3019-3030.
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