杨梅中农药残留检测技术及仙居县杨梅产业发展分析
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摘要
仙居县是浙江省乃至全国的杨梅主产区之一,仙居杨梅具有“绿色无公害水果”之美誉。但仍不少农户违反规定在杨梅成熟期治虫导致农药残留问题突出,果实品质降低。严重的农药残留问题给该县杨梅的质量安全带来潜在的隐患,给仙居杨梅走向国际化带来巨大的困难,更给仙居杨梅产业的可持续发展带来严峻的考验。
为了有效控制农药在杨梅生产中的合理使用和对其残留量进行监控,满足进出口贸易的需要,同时促进仙居杨梅产业保持快速、健康发展,本论文以仙居产荸荠种杨梅和东魁杨梅为原料,对可能用于杨梅生产过程杨梅中的有机磷类、有机氯类及拟除虫聚酯类农药进行残留量进行定性、定量分析检测研究,并分析了仙居县杨梅产业发展的特点及存在的问题,提出仙居县杨梅产业发展的建议和对策。主要结论如下:
(1)建立了固相萃取-气相色谱法测定杨梅中有机磷类农药残留的检测方法。对杨梅中有机磷类农药残留的提取方法进行了探讨研究。采用本方法,在给定色谱条件下,甲胺磷、敌敌畏、甲拌磷、毒死蜱、对硫磷、乙酰甲胺磷、氧化乐果、久效磷、磷胺、杀螟硫磷、水胺硫磷、三唑磷、甲基对硫磷等13种有机磷农药能达到良好分离,目标回收率在72.1%~95.3%之间,相对标准偏差(RSD)在2.38%~10.4%之间,回收率较稳定。
(2)建立了固相萃取-气相色谱法测定杨梅中有机氯类及拟除虫聚酯类农药残留的检测方法。对杨梅中有机氯和拟除虫菊酯类农药残留的提取方法进行了探讨,并对固相萃取浓缩净化的条件进行了选择。在给定色谱条件下,氯氰菊酯、氰戊菊酯、溴氰菊酯、甲氰菊酯、联苯菊酯、氟氯氰菊酯、氯氟氰菊酯、百菌清、三唑酮等9种农药能达到良好分离,平均回收率在71.2%~91.1%之间,相对标准偏差在2.32%~10.13%之间,具有稳定的回收率。
(3)建立了杨梅中农药残留快速检测的方法。采用酶抑制法对仙居产荸荠种杨梅进行水胺硫磷、乐果、氧化乐果、敌敌畏、毒死蜱、甲胺磷、对硫磷、杀螟硫磷、敌百虫等9种农药进行检测,将检测所得酶抑制率和添加水平结果进行对比分析。检测结果显示,在添加同一浓度同一种有机磷农药时,相对标准偏差均在9%以下,酶抑制率相对比较稳定。在添加浓度达到1mg/kg时,酶抑制率检测结果均达到50%以上,可判断为阳性。
(4)分析了仙居杨梅产业发展的特点,包括发展速度快、致富速度快、具有品牌优势、快速带动其他产业发展等方面;总结了仙居杨梅产业在发展中存在的主要问题,如日益突出的农药残留问题、自然灾害影响严重、杨梅基地基础设施薄弱、杨梅品牌建设和保护深化存在一定困难等。并提出杨梅产业发展建议和对策:一是全面推行检测制度,确保杨梅质量安全;二是推行绿色防控和生态栽培,加大农业投入品监管力度;二是加强基础设施和市场体系建设,改善杨梅生产和销售条件;三是加大仙居杨梅品牌打假力度,规范市场营销秩序;四是加强杨梅产后研究,推动杨梅产业发展。
Xianju County is main producing areas of Myrica rubra Sieb.et Zucc. in Zhejiang Province and the whole country, also Xianju bayberry has a reputation of "pollution-free fruits and green". Many farmers are still breaking rules by controlling pest during period of bayberry maturity, which cause serious problems of pesticide residues and decreasing fruit quality. Serious problem of pesticide residues in the quality and safety bring the county bayberry potential pitfalls, and enormous difficulties of Xianju Bayberry internationalization, but also serious challenges of the sustainable development of Xianju bayberry industry.
In order to effectively control the rational use of pesticides in bayberry’s production and to monitor their residues, to meet the needs of import and export trade, also promoting Xianju Bayberry industry to maintain rapid, healthy development, this thesis uses Biqi bayberry and Dongkui Bayberry as raw materials, qualitative and quantitative analysis of detection the organophosphate, organochlorine pesticides and polyester pesticides residues in production processes of bayberry, and analysis of industrial development Xianju bayberry Characteristics and problems of industrial development proposed suggestions and countermeasures of Xianju bayberry industry. The main conclusions are as follows:
(1) Solid phase extraction– use gas chromatography to detect the organophosphorus pesticide residues in Bayberry. Discuss the method of extraction Organic phosphorus of bayberry pesticide residues. By this method in a given chromatographic conditions, methamidophos, dichlorvos, phorate, chlorpyrifos, parathion, acephate, omethoate, monocrotophos, phosphorus amine, fenitrothion, water, amines Parathion, triazophos, methyl parathion etc.13 kinds of organophosphorus pesticides could achieve good separation, the target recovery was 72.1% ~ 95.3%, the relative standard deviation (RSD) 2.38%~10.4%, and recovery was more stable.
(2) Solid phase extraction– use gas chromatography to detect bayberry’s Organochlorine pesticides and the pyrethroi pesticides. Discussed the extraction methods of bayberry’s organochlorine and pyrethroi pesticides residues, and the purification of solid phase extraction enrichment conditions were selected. Under the given chromatographic conditions, cypermethrin, fenvalerate, deltamethrin, fenpropathrin, bifenthrin, cyfluthrin, cyhalothrin, chlorothalonil, triadimefon etc. 9 kinds of pesticides could achieve good separation, the average recovery was 71.2% ~ 91.1% with relative standard deviations between 2.32% ~ 10.13%, with a stable recovery.
(3) Establish a method of a rapid detection of pesticide residues in bayberry. Detect isocarbophos, dimethoate, omethoate, dichlorvos, chlorpyrifos, parathion, methamidophos, fenitrothion, trichlorfon etc. 9 kinds of pesticides from Xianju Biqi bayberry via enzyme inhibition method which compared the detected the income level of enzyme inhibition rate and add the results. Test results showed that adding the same concentration with an organic phosphorus pesticide, the relative standard deviations were below 9%, inhibition rate was relatively stable. When adding concentration of 1mg/kg, enzyme inhibition test results were up to 50%, judged as positive.
(4) analyzed the characteristics of Xianju bayberry industrial development, including the fast development, getting rich quick, with a brand, promoting rapid development of other industries, etc.; summarizes major problems of the Xianju bayberry industry’s development, such as increasing the issue of pesticide residues, serious natural disasters, weak infrastructure of bayberry base, some difficulties in brand building and protection. And here some suggestions and measures for Bayberry industry: First, full implementation of the testing system to ensure bayberry’s quality and safety; Second, the implementation of prevention and control of green and ecological cultivation, increasing inputs of supervision of agricultural; Third, strengthen the infrastructure and market system, improve bayberry production and sales conditions; Fourth, increase efforts to crack down fake Xianju Bayberry brand and standardize the market order; Fifth, strengthen post-natal study of bayberry, promoting industrial development.
为了有效控制农药在杨梅生产中的合理使用和对其残留量进行监控,满足进出口贸易的需要,同时促进仙居杨梅产业保持快速、健康发展,本论文以仙居产荸荠种杨梅和东魁杨梅为原料,对可能用于杨梅生产过程杨梅中的有机磷类、有机氯类及拟除虫聚酯类农药进行残留量进行定性、定量分析检测研究,并分析了仙居县杨梅产业发展的特点及存在的问题,提出仙居县杨梅产业发展的建议和对策。主要结论如下:
(1)建立了固相萃取-气相色谱法测定杨梅中有机磷类农药残留的检测方法。对杨梅中有机磷类农药残留的提取方法进行了探讨研究。采用本方法,在给定色谱条件下,甲胺磷、敌敌畏、甲拌磷、毒死蜱、对硫磷、乙酰甲胺磷、氧化乐果、久效磷、磷胺、杀螟硫磷、水胺硫磷、三唑磷、甲基对硫磷等13种有机磷农药能达到良好分离,目标回收率在72.1%~95.3%之间,相对标准偏差(RSD)在2.38%~10.4%之间,回收率较稳定。
(2)建立了固相萃取-气相色谱法测定杨梅中有机氯类及拟除虫聚酯类农药残留的检测方法。对杨梅中有机氯和拟除虫菊酯类农药残留的提取方法进行了探讨,并对固相萃取浓缩净化的条件进行了选择。在给定色谱条件下,氯氰菊酯、氰戊菊酯、溴氰菊酯、甲氰菊酯、联苯菊酯、氟氯氰菊酯、氯氟氰菊酯、百菌清、三唑酮等9种农药能达到良好分离,平均回收率在71.2%~91.1%之间,相对标准偏差在2.32%~10.13%之间,具有稳定的回收率。
(3)建立了杨梅中农药残留快速检测的方法。采用酶抑制法对仙居产荸荠种杨梅进行水胺硫磷、乐果、氧化乐果、敌敌畏、毒死蜱、甲胺磷、对硫磷、杀螟硫磷、敌百虫等9种农药进行检测,将检测所得酶抑制率和添加水平结果进行对比分析。检测结果显示,在添加同一浓度同一种有机磷农药时,相对标准偏差均在9%以下,酶抑制率相对比较稳定。在添加浓度达到1mg/kg时,酶抑制率检测结果均达到50%以上,可判断为阳性。
(4)分析了仙居杨梅产业发展的特点,包括发展速度快、致富速度快、具有品牌优势、快速带动其他产业发展等方面;总结了仙居杨梅产业在发展中存在的主要问题,如日益突出的农药残留问题、自然灾害影响严重、杨梅基地基础设施薄弱、杨梅品牌建设和保护深化存在一定困难等。并提出杨梅产业发展建议和对策:一是全面推行检测制度,确保杨梅质量安全;二是推行绿色防控和生态栽培,加大农业投入品监管力度;二是加强基础设施和市场体系建设,改善杨梅生产和销售条件;三是加大仙居杨梅品牌打假力度,规范市场营销秩序;四是加强杨梅产后研究,推动杨梅产业发展。
Xianju County is main producing areas of Myrica rubra Sieb.et Zucc. in Zhejiang Province and the whole country, also Xianju bayberry has a reputation of "pollution-free fruits and green". Many farmers are still breaking rules by controlling pest during period of bayberry maturity, which cause serious problems of pesticide residues and decreasing fruit quality. Serious problem of pesticide residues in the quality and safety bring the county bayberry potential pitfalls, and enormous difficulties of Xianju Bayberry internationalization, but also serious challenges of the sustainable development of Xianju bayberry industry.
In order to effectively control the rational use of pesticides in bayberry’s production and to monitor their residues, to meet the needs of import and export trade, also promoting Xianju Bayberry industry to maintain rapid, healthy development, this thesis uses Biqi bayberry and Dongkui Bayberry as raw materials, qualitative and quantitative analysis of detection the organophosphate, organochlorine pesticides and polyester pesticides residues in production processes of bayberry, and analysis of industrial development Xianju bayberry Characteristics and problems of industrial development proposed suggestions and countermeasures of Xianju bayberry industry. The main conclusions are as follows:
(1) Solid phase extraction– use gas chromatography to detect the organophosphorus pesticide residues in Bayberry. Discuss the method of extraction Organic phosphorus of bayberry pesticide residues. By this method in a given chromatographic conditions, methamidophos, dichlorvos, phorate, chlorpyrifos, parathion, acephate, omethoate, monocrotophos, phosphorus amine, fenitrothion, water, amines Parathion, triazophos, methyl parathion etc.13 kinds of organophosphorus pesticides could achieve good separation, the target recovery was 72.1% ~ 95.3%, the relative standard deviation (RSD) 2.38%~10.4%, and recovery was more stable.
(2) Solid phase extraction– use gas chromatography to detect bayberry’s Organochlorine pesticides and the pyrethroi pesticides. Discussed the extraction methods of bayberry’s organochlorine and pyrethroi pesticides residues, and the purification of solid phase extraction enrichment conditions were selected. Under the given chromatographic conditions, cypermethrin, fenvalerate, deltamethrin, fenpropathrin, bifenthrin, cyfluthrin, cyhalothrin, chlorothalonil, triadimefon etc. 9 kinds of pesticides could achieve good separation, the average recovery was 71.2% ~ 91.1% with relative standard deviations between 2.32% ~ 10.13%, with a stable recovery.
(3) Establish a method of a rapid detection of pesticide residues in bayberry. Detect isocarbophos, dimethoate, omethoate, dichlorvos, chlorpyrifos, parathion, methamidophos, fenitrothion, trichlorfon etc. 9 kinds of pesticides from Xianju Biqi bayberry via enzyme inhibition method which compared the detected the income level of enzyme inhibition rate and add the results. Test results showed that adding the same concentration with an organic phosphorus pesticide, the relative standard deviations were below 9%, inhibition rate was relatively stable. When adding concentration of 1mg/kg, enzyme inhibition test results were up to 50%, judged as positive.
(4) analyzed the characteristics of Xianju bayberry industrial development, including the fast development, getting rich quick, with a brand, promoting rapid development of other industries, etc.; summarizes major problems of the Xianju bayberry industry’s development, such as increasing the issue of pesticide residues, serious natural disasters, weak infrastructure of bayberry base, some difficulties in brand building and protection. And here some suggestions and measures for Bayberry industry: First, full implementation of the testing system to ensure bayberry’s quality and safety; Second, the implementation of prevention and control of green and ecological cultivation, increasing inputs of supervision of agricultural; Third, strengthen the infrastructure and market system, improve bayberry production and sales conditions; Fourth, increase efforts to crack down fake Xianju Bayberry brand and standardize the market order; Fifth, strengthen post-natal study of bayberry, promoting industrial development.
引文
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GB/T 5009.145-2003植物性食品中有机磷和氨基甲酸酯类农药多种残留的测定
GB/T 5009.146-2003植物性食品中有机氯和拟除虫菊酯类农药多种残留的测定
NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定
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GB/T 5009.145-2003植物性食品中有机磷和氨基甲酸酯类农药多种残留的测定
GB/T 5009.146-2003植物性食品中有机氯和拟除虫菊酯类农药多种残留的测定
NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定
Javier R L,Cesar O F,Pedro W E.Changes in anthocyanin concentration in lychee (1itchi chinensis sonn.) pericarp during maturation.Food Chem,1999,65:195-200