吐温-80增敏同步荧光法检测蔬菜中二甲菌核利残留
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摘要
基于表面活性剂可增强二甲菌核利荧光强度,建立同步荧光分光光度法测定蔬菜中二甲菌核利残留量。对波长差进行了优化;讨论了溶剂种类、缓冲液的种类、用量及pH值等因素对二甲菌核利荧光强度的影响;应用正交实验对提取剂种类、用量、超声时间进行优化。选择甲醇做溶剂和提取剂,质量浓度为4.29 g?L~(-1)吐温-80做表面活性剂。在0.14～3.00μg?mL~(-1)范围内,二甲菌核利浓度与荧光强度线性关系良好,检出限为0.105 6 mg?kg~(-1),回收率为82.63～99.77%,RSD为0.16～0.61%。
Synchronous fluorescence method for determining pythium residues in vegetables based on surfactants sensitization was developed.The wavelength difference(Δλ)was selected.The effect of the solvent type,the type and amount of buffer,pH on the fluorescence intensity was discussed.The type and dosage of the extractant,the ultrasonic time were optimized by orthogonal test.Methanol was used as solvent and extractant.Tween-80(4.29 g?L~(-1))was used as the surfactant.In the range of 0.14 to 3.00μg?mL~(-1),the linear relationship between the concentration of pythium and its fluorescence intensity was good,and the detection limit was 0.105 6 mg?kg~(-1).The recovery were 82.63 to 99.77%,RSD was 0.16 to 0.61%.The new method can be used to determine pythium residues in vegetables.
Synchronous fluorescence method for determining pythium residues in vegetables based on surfactants sensitization was developed.The wavelength difference(Δλ)was selected.The effect of the solvent type,the type and amount of buffer,pH on the fluorescence intensity was discussed.The type and dosage of the extractant,the ultrasonic time were optimized by orthogonal test.Methanol was used as solvent and extractant.Tween-80(4.29 g?L~(-1))was used as the surfactant.In the range of 0.14 to 3.00μg?mL~(-1),the linear relationship between the concentration of pythium and its fluorescence intensity was good,and the detection limit was 0.105 6 mg?kg~(-1).The recovery were 82.63 to 99.77%,RSD was 0.16 to 0.61%.The new method can be used to determine pythium residues in vegetables.
引文
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[2]张群,吴南村,张月,等.气相色谱-串联质谱法测定韭菜中的三唑酮和腐霉利残留[J].农药学学报,2016,18(3):397-401.
[3]孙通,莫欣欣,李晓珍,等.近红外光谱技术结合变量选择方法定性检测食用植物油中的腐霉利[J].光谱学与光谱分析,2016,36(12):3915-3919.
[4]食品中农药最大残留限量(GB2763-2016)[S].北京:中国标准出版社,2017.
[5]水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法(GB23200.8-2016)[S].北京:中国标准出版社,2017.
[6]Araujo E A,Lara M C R,Reis M R D,et al.Determination of Haloxyfop-Methyl,Linuron,and Procymidone Pesticides in Carrot Using SLE-LTPExtraction and GC-MS[J].Food Anal.Methods,2016,9(5):1344-1352.
[7]Chu S P,Tseng W C,Kong P H,et al.Up-and-DownShaker-Assisted Dispersive Liquid-Liquid Microextration Coupled with Gas Chromatography-Mass Spectrometry for the Determination of Fungicides in Wine[J].Food Chemistry,2015,185:377-382.
[8]胡祥娜,顾亚萍,林慧纯,等.高效液相色谱串联四极杆质谱法同时测定豆芽中7种药物残留[J].食品科学,2014,35(20):253-257.
[9]Juan-Garcia A,Font G,Pico Y.Quantitative Analysis of Six Pesticides in Fruits by Capillary Electrophoresis Electrospray-Mass Spectrometry[J].Electrophoresis,2005,26(7-8):1550-1561.
[10]Rodiguez R,Pico Y,Font G,et al.Analysis of Thiabendazole and Procymidone in Fruits and Vegetables by Capillary Electrophoresis-Electrospray Mass Spectrometry[J].Journal of Chromatography A,2002,949(1-2):359-366.
[11]Tuzimski T,Rejczak T.Determination of Pesticides in Sunflower Seeds by High-Performance Liquid Chromatography Coupled with a Diode Array Detector[J].J AOAC Int,2014,97(4):1012-1020.
[12]Xu Z,Huan Z B,Luo J H,et al.Simultaneous Determination of Eight Pesticide Residues in Cowpeas by GC-ECD[J].J Chromatogr Sci,2017,55(1):1-6.
[13]Fulgencio A C D C,Saczk A A,Oliveira M F D,et al.New Voltammetry-Based Analytical Method for Indirect Determination of Procymidone in Brazilian Apples[J].Food Anal Methods,2014,7(1):31-38.
[14]Frenandez-Albaa R,Valverde A,Aguera A,et al.Determination of Procymidone in Vegetables by a Commercial Competitive Inhibition Enzyme Immunoassay[J].Analytica Chimica Acta,1995,311(3):371-376.
[15]刘宇.仪器分析[M].天津:天津大学出版社,2010:137.
[16]齐畅,刘美欧,杨珊珊,等.分散液相微萃取荧光法测定果蔬中残留吡蚜酮[J].农药,2017,56(6):434-436.