超声辅助溶剂萃取结合反相高压液相色谱法检测番茄果实中丙烷脒杀菌剂残留分析研究
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摘要
丙烷脒作为一个系统性植物病害防治剂，被广泛应用于大田或大棚果蔬上由灰葡萄孢引起的病害。丙烷脒的毒性低，对人类和环境安全。然而，至今没有丙烷脒在植物上的残留的研究报道。因此，对丙烷脒在番茄上的残留试验便显得尤为重要。
本研究尝试建立一种丙烷脒在番茄上的残留检验方法。装有两种填料（5μm和10μm）的Hypersil BDS C18色谱柱(4.6mm×250mm)被分别应用在反相高效液相色谱（RP-HPLC）上。共用了三种萃取溶剂，甲醇、磷酸化甲醇和HCL PBS溶液，在超声辅助下分别对样品进行丙烷脒提取。测定方法被验证可用于残留分析。
通过试验，流动相组分为0.1%磷酸(H3PO4)，甲醇/去离子水（V/V=80:20）溶液含3.0mmol/L SDS时丙烷脒的分析信号值达到最大。通过超声辅助将番茄中的丙烷脒提取出来。样品上样至HPLC系统中，10μm Hypersil BDS C18柱(4.6mm×250mm)等梯度流速1.0ml/min，柱温25oC。进样20μl，于262nm下检测。这一方法在50~600mg/L的浓度范围内的线性良好，相关系数>0.999。回收率为87.97%~106.34%（标准差：0.169%~3.503%）。检测限和定量限分别为0.07mg/Kg和0.2mg/Kg。
田间用药试验于中国西北农林科技大学无公害农药研究服务中心的玻璃温室和位于大学区十五公里的小寨（中国陕西杨凌）的阳光温室内进行。初始丙烷脒浓度在玻璃温室和阳光温室内分别设置为4.69~2.87mg/Kg和5.70~2.45mg/Kg。丙烷脒的分解呈一级动力学，与初始存量、浓度和用药次数均无关。在玻璃温室内的分解半衰期为5.331~7.875天，在阳光温室则为4.880~6.300天。
28天后丙烷脒残留为0.07mg/Kg，开始低于检测限。结果表明这一方法对丙烷脒残留检测定量的可行性。由试验得到的数据证明了这一方法会在丙烷脒MRL的建立和常规残留检测得到应用。
与其他的杀菌剂检测方法相比，超声辅助和溶剂萃取结合反相高效液相色谱的方法显得更简单、快捷、有效和便宜。
Propamidine is a novel systemic plant fungicide which is mainly used to control variousdiseases caused by botrytis fungi on fruits and vegetables under field and greenhouseconditions. It was reported that propamidine is of low toxicity, safe to human being andenvironment. However, no published data are available concerning the residues ofpropamidine in plant extracts. Therefore, residual analysis study of propamidine in tomatobecomes indispensable to guarantee the use of propamidine in field according to goodagricultural practices.
The present study is the first attempt for determination and validation of a method forpropamidine residues in tomato fruits. A method of reverse phase high performance liquidchromatography (RP-HPLC) UV detection using two types (5μm and10μm) of HypersilBDS C18column (4.6mm×250mm) was tested. The extraction of propamidine was basedon ultrasonic assisted solvent extraction using an extracting solvent including pure methanol,methanol acidified with phosphoric acid, and HCl-PBS solution. The determinate method wasvalidated and used for propamidine residues quantification in the residues kinetic dissipationstudy.
For method determination the best analytical signals response of propamidine fungicidewas achieved with a mobile phase consisting of0.1%phosphoric acid (H3PO4), methanol/de-ionized water (V/V=80:20) solution containing3.0mmol/L SDS. Propamidine was extractfrom tomato fortified and real samples using an ultrasound-assisted solvent extraction. Thesamples were analyzed using reverse phase high performance liquid chromatography with10μm Hypersil BDS C18column (4.6mm×250mm) at the flow rate of1.0ml/min and thecolumn temperature of25oC; injection volume was20μl and the UV detector wavelength wasset at262nm using an isocratic elution system. The method was validated with good linearityin the concentration range of50–600mg/L with determination coefficient>0.999.Satisfactory recoveries ranged from87.97to106.34%with relative standard deviations between0.169and3.503%were obtained for fortified samples. The detection limit andquantification limit were0.07mg/Kg and0.2mg/Kg respectively.
For the dissipation study the experimental trials were conducted in a glasshouse atResearch&Development Center of Biorational pesticide (RDCBP), Northwest A&FUniversity, China and in solar greenhouse condition at the village of Xiao-zai (Shaanxi, China)located at fifteen kilometer in the west of Northwest A&F University. The initial depositranged from4.69to2.87mg/Kg and5.70to2.45mg/Kg for all treatments respectively in thetrial of glasshouse and greenhouse. The dissipation of propamidine was found to be first-orderkinetics dissipation, independent of the initial deposit, application dose and the number ofapplication in both environments (glasshouse and greenhouse). The corresponding half-liveranged from5.331to7.875days in glasshouse trial and4.880to6.300days in greenhouse.These propamidine residues dissipated below the limit of detection of0.07mg/Kg28daysafter the last treatment in both cases. The results found were acceptable and confirmed thatthe method is suitable for propamidine residues quantification. The residues data from realsamples carried out in glasshouse and greenhouse tomato had proved that the method could beuseful for the establishment of MRL of propamidine and routine residues analysis.
Compared to other method used in pesticide determination, the Ultrasound-AssistedSolvent Extraction Method using Reserve Phase High Pressure Liquid Chromatographydeterminate and validated in this work is easy, quick, efficient and no expansive.
本研究尝试建立一种丙烷脒在番茄上的残留检验方法。装有两种填料（5μm和10μm）的Hypersil BDS C18色谱柱(4.6mm×250mm)被分别应用在反相高效液相色谱（RP-HPLC）上。共用了三种萃取溶剂，甲醇、磷酸化甲醇和HCL PBS溶液，在超声辅助下分别对样品进行丙烷脒提取。测定方法被验证可用于残留分析。
通过试验，流动相组分为0.1%磷酸(H3PO4)，甲醇/去离子水（V/V=80:20）溶液含3.0mmol/L SDS时丙烷脒的分析信号值达到最大。通过超声辅助将番茄中的丙烷脒提取出来。样品上样至HPLC系统中，10μm Hypersil BDS C18柱(4.6mm×250mm)等梯度流速1.0ml/min，柱温25oC。进样20μl，于262nm下检测。这一方法在50~600mg/L的浓度范围内的线性良好，相关系数>0.999。回收率为87.97%~106.34%（标准差：0.169%~3.503%）。检测限和定量限分别为0.07mg/Kg和0.2mg/Kg。
田间用药试验于中国西北农林科技大学无公害农药研究服务中心的玻璃温室和位于大学区十五公里的小寨（中国陕西杨凌）的阳光温室内进行。初始丙烷脒浓度在玻璃温室和阳光温室内分别设置为4.69~2.87mg/Kg和5.70~2.45mg/Kg。丙烷脒的分解呈一级动力学，与初始存量、浓度和用药次数均无关。在玻璃温室内的分解半衰期为5.331~7.875天，在阳光温室则为4.880~6.300天。
28天后丙烷脒残留为0.07mg/Kg，开始低于检测限。结果表明这一方法对丙烷脒残留检测定量的可行性。由试验得到的数据证明了这一方法会在丙烷脒MRL的建立和常规残留检测得到应用。
与其他的杀菌剂检测方法相比，超声辅助和溶剂萃取结合反相高效液相色谱的方法显得更简单、快捷、有效和便宜。
Propamidine is a novel systemic plant fungicide which is mainly used to control variousdiseases caused by botrytis fungi on fruits and vegetables under field and greenhouseconditions. It was reported that propamidine is of low toxicity, safe to human being andenvironment. However, no published data are available concerning the residues ofpropamidine in plant extracts. Therefore, residual analysis study of propamidine in tomatobecomes indispensable to guarantee the use of propamidine in field according to goodagricultural practices.
The present study is the first attempt for determination and validation of a method forpropamidine residues in tomato fruits. A method of reverse phase high performance liquidchromatography (RP-HPLC) UV detection using two types (5μm and10μm) of HypersilBDS C18column (4.6mm×250mm) was tested. The extraction of propamidine was basedon ultrasonic assisted solvent extraction using an extracting solvent including pure methanol,methanol acidified with phosphoric acid, and HCl-PBS solution. The determinate method wasvalidated and used for propamidine residues quantification in the residues kinetic dissipationstudy.
For method determination the best analytical signals response of propamidine fungicidewas achieved with a mobile phase consisting of0.1%phosphoric acid (H3PO4), methanol/de-ionized water (V/V=80:20) solution containing3.0mmol/L SDS. Propamidine was extractfrom tomato fortified and real samples using an ultrasound-assisted solvent extraction. Thesamples were analyzed using reverse phase high performance liquid chromatography with10μm Hypersil BDS C18column (4.6mm×250mm) at the flow rate of1.0ml/min and thecolumn temperature of25oC; injection volume was20μl and the UV detector wavelength wasset at262nm using an isocratic elution system. The method was validated with good linearityin the concentration range of50–600mg/L with determination coefficient>0.999.Satisfactory recoveries ranged from87.97to106.34%with relative standard deviations between0.169and3.503%were obtained for fortified samples. The detection limit andquantification limit were0.07mg/Kg and0.2mg/Kg respectively.
For the dissipation study the experimental trials were conducted in a glasshouse atResearch&Development Center of Biorational pesticide (RDCBP), Northwest A&FUniversity, China and in solar greenhouse condition at the village of Xiao-zai (Shaanxi, China)located at fifteen kilometer in the west of Northwest A&F University. The initial depositranged from4.69to2.87mg/Kg and5.70to2.45mg/Kg for all treatments respectively in thetrial of glasshouse and greenhouse. The dissipation of propamidine was found to be first-orderkinetics dissipation, independent of the initial deposit, application dose and the number ofapplication in both environments (glasshouse and greenhouse). The corresponding half-liveranged from5.331to7.875days in glasshouse trial and4.880to6.300days in greenhouse.These propamidine residues dissipated below the limit of detection of0.07mg/Kg28daysafter the last treatment in both cases. The results found were acceptable and confirmed thatthe method is suitable for propamidine residues quantification. The residues data from realsamples carried out in glasshouse and greenhouse tomato had proved that the method could beuseful for the establishment of MRL of propamidine and routine residues analysis.
Compared to other method used in pesticide determination, the Ultrasound-AssistedSolvent Extraction Method using Reserve Phase High Pressure Liquid Chromatographydeterminate and validated in this work is easy, quick, efficient and no expansive.
引文
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