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《化学分析计量》 2019年第03期
DOI:10.3969/j.issn.1008-6145.2019.03.009
固相萃取-气相色谱-串联质谱法测定甘蓝类蔬菜中氟啶虫酰胺和嘧菌环胺
曹建涛1,毕思远24,田伟1,巩少岩3,曹涛4,朱志强2
1. 济南市农产品质量检测中心,济南 250000; 2. 哈尔滨体育学院滑雪教学训练基地,哈尔滨 150008;
3. 济南护理职业学院,济南 250102; 4. 广东省检迅检测科技有限公司,广东 
Determination of fluridinamide and cyprodinil in cabbage vegetables by solid phase extraction-gas chromatography-tandem mass spectrometry
CAO Jiantao1, BI Siyuan2,4, TIAN Wei1, GONG Shaoyan3, CAO Tao4, ZHU Zhiqiang2
1. Jinan Test Center for Agri-products Quality, Jinan 250000, China;
2. Ski Teaching and Training Base Post–doctoral Research Station of Harbin Sport University, Harbin 150008, China;
3. Jinan Vocational College of Nursing, Jinan 250102, China;
4. Guangdong Quick Test Technologies Co., Ltd., Dongguan 523843, China 
摘要:建立固相萃取-气相色谱-串联质谱(GC-MS-MS) 测定甘蓝类蔬菜中氟啶虫酰胺和嘧菌环胺残留量的分析方法。甘蓝类蔬菜样品经乙腈提取后,用ENVI-Carb 活性炭固相萃取柱净化,乙腈-甲苯(3∶1) 溶液进行洗脱,采用GC-MS-MS 法测定,以保留时间和选择性反应监测(MRM) 离子对定性,色谱峰面积定量。氟啶虫酰胺和嘧菌环胺的质量浓度在0.05~2.0 μg/mL 范围内与色谱峰面积呈良好的线性关系,线性相关系数均大于0.998,检出限分别为0.005,0.008 mg/kg。样品加标回收率为87.4%~97.3%,测定结果的相对标准偏差为1.3%~3.2%(n=6)。该方法灵敏度和准确度高,适用于甘蓝类蔬菜中氟啶虫酰胺和嘧菌环胺残留的测定。 
Abstract:A method for the determination of fluridinamide and cyprodinil in cabbage vegetables by solid phase extraction-gas chromatography-tandem mass spectrometry (GC-MS-MS) was established. The samples of cabbage vegetables were extracted by acetonitrile, extracted solution was purified by ENVI-Carb activated carbon solid phase extraction column, eluted by acetonitrile-toluene (3:1) solution, and determined by GC-MS-MS. Retention time and selective reaction monitoring (MRM) ion pair were determined qualitatively and chromatographic peak area quantitatively determinated. The mass concentration of fluridinamide and cyprodinil had good linear relationship with its chromatographic peak area in the range of 0.05-2.0 μg/mL. The linear correlation coefficients were more than 0.998. The detection limits were 0.005 and 0.008 mg/kg, respectively. The average recoveries of samples were ranged 87.4%-97.3%. The relative standard deviation of the determination results were 1.3%-3.2%(n=6). The method has high sensitivity and accuracy, it is suitable for the detection of fluridinamide and cyprodinil in cabbage vegetables. 
关键词:固相萃取;气相色谱-串联质谱法;氟啶虫酰胺;嘧菌环胺;甘蓝 
Keywords:solid phase extraction; gas chromatography-tandem mass spectrometry; fluridinamide; cyprodinil;cabbage 
基金:国家博士后基金面上项目二等资助(No. 2017M611382) 
本文引用格式:
曹建涛,毕思远,田伟,等. 固相萃取- 气相色谱- 串联质谱法测定甘蓝类蔬菜中氟啶虫酰胺和嘧菌环胺[J]. 化学分析计量,2019,28(3):34-37.
CAO J T,BI S Y,TIAN W,et al. Determination of fluridinamide and cyprodinil in cabbage vegetables by solid phase extraction-gas chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage,2019,28(3):34-37. 

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