CN105021436B - 一种农药提取液及其应用 - Google Patents
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Abstract
本发明公开了一种农药提取液及其应用，由磷酸盐或碳酸盐和醇类混合而成，用于提取动植物材料、食品、饮品、土壤中的农药残留，无需调节pH﹑过层析柱以及氧化等复杂的样品前处理过程，即可应用于样品中的农药快速残留检测，所用试剂安全环保且用量少。
Description
技术领域
本发明属于分析化学领域，具体涉及一种农药提取液及其应用。
背景技术
在农药残留快速检测中，从实验样品中提取出残留农药是一个很关键的步骤，对于许多动植物材料、食品等样品，因其本身含有许多会影响酶抑制反应的内源物质，因此在前期的农药残留快速检测方法中一般都使用较复杂的提取方法，如在推荐性的国家标准GB/T18625-2002《茶中有机磷及氨基甲酸酯农药残留量的简易检验方法酶抑制法》中，对茶叶样品中的农药的提取就需要在样品加入一定量的丙酮进行浸泡后，再加入碳酸钙以去除对酶抑制反应有影响的干扰物质；有的方法是将样品用试剂浸泡提取后用酸度调节剂调节PH在4~5之间后再过层析柱处理以排除干扰物质。农药的提取方法冗长繁杂、并且耗费大量有机试剂并增加实验人员的工作量，有机溶剂的大量使用不仅损害实验人员身体健康而且对环境也同样存在着污染。
发明内容
本发明的目的在于提供一种农药提取液及其应用，用于提取动植物材料、食品、饮品、土壤中的中的农药残留，无需调节pH﹑过层析柱以及氧化过程，所用试剂安全环保且用量少。
为实现上述目的，本发明采用如下技术方案：
一种农药提取液，由磷酸盐或碳酸盐和醇类混合而成。
在20～80mL磷酸盐或碳酸盐缓冲溶液中加入50～300mL丙三醇混匀后，再加入100～300mL95wt.%乙醇溶液摇匀。
所述的农药提取液用于动植物材料、食品、饮品、土壤中的有机磷和氨基甲酸酯类农药残留检测。
本发明的显著优点在于：本发明制得的农药提取液用于提取动植物材料、食品、饮品、土壤中的中的农药残留，无需调节pH﹑过层析柱以及氧化过程等复杂的样品前处理过程，即可应用于样品中的农药残留快速检测，所用试剂安全环保且用量少。
具体实施方式
实施例1
一种茶叶或茶青中农药残留的检测方法：茶叶或茶青中有机磷和氨基甲酸酯类农药残留的检测步骤：
（1）试剂的配制：
Et试剂：无需配制，直接开封启用；所述的Et试剂的为胆碱酯酶和5,5'-二硫代双(2-硝基苯甲酸)的混合液，两者的重量比为1︰40～100。
Sub试剂：在10 mL蒸馏水中加入10-60mg碘化硫代乙酰胆碱，摇匀使之溶解；
农药提取液：在20～80mL磷酸盐或碳酸盐缓冲溶液中加入50～300mL丙三醇，混匀后再加入100～300mL95wt.%乙醇溶液，混匀；
缓冲液：在500mL蒸馏水中加入5～15g磷酸氢二钠和0.2～0.8g磷酸二氢钾，混匀；
（2）检测
样品提取：
称取0.5g茶叶样品，加入1.0mL农药提取液，使样品充分浸润并静置10分钟，底部溶液即为待测液；
对照测定：
吸取Et试剂100μL，加入1.5mL缓冲液，摇匀，加入200μL提取液，摇匀，静置10分钟，加入100μL Sub试剂，摇匀后移入0.5cm比色皿，及时放入农药残留测试仪上进行对照测试；
样品测定：
吸取Et试剂100μL，加入1.5mL缓冲液，摇匀，加入200μL待测液，摇匀，静置10分钟，加入100μLSub试剂，摇匀后移入0.5cm比色皿，及时放入农药残留测试仪上进行样品测试；
测定结果的判定：
当检测结果的酶抑制率读数超过50%时，表明样品农药残留毒性可能超过安全标准，应当确认操作步骤无误、仪器工作正常、试剂没有污染失效，重新进行对照测试并对此样品进行2次以上的重复检测，如检测结果重复并仍然超过50%，则需用气相色谱作进一步的确认。
应用上述所发明的农药提取液，在铁观音茶叶和实验室栽种的无农药的茶青进行农药加样提取测定，得到的不同农药的检测灵敏度如下：
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (1)
1. 一种农药提取液的应用，其特征在于：由磷酸盐或碳酸盐和醇类混合而成；在20～80mL 磷酸盐或碳酸盐缓冲溶液中加入50～300mL 丙三醇混匀后，再加入100～300mL95wt.% 乙醇溶液摇匀；所述的农药提取液用于茶叶或茶青的农药残留检测；茶叶或茶青中有机磷和氨基甲酸酯类农药残留的检测步骤：
（1）试剂的配制：
Et 试剂：无需配制，直接开封启用；所述的Et 试剂的为胆碱酯酶和5,5'-二硫代双-2-硝基苯甲酸的混合液，两者的重量比为1︰40～100；
Sub 试剂：在10 mL 蒸馏水中加入10-60mg 碘化硫代乙酰胆碱，摇匀使之溶解；
农药提取液：在20～80mL 磷酸盐或碳酸盐缓冲溶液中加入50～300mL 丙三醇，混匀后再加入100～300mL95wt.%乙醇溶液，混匀；
缓冲液：在500mL 蒸馏水中加入5～15g 磷酸氢二钠和0.2～0.8g 磷酸二氢钾，混匀；
（2）检测
样品提取：
称取0.5g 茶叶样品，加入1.0mL 农药提取液，使样品充分浸润并静置10 分钟，底部溶液即为待测液；
对照测定：
吸取Et试剂100μL，加入1.5mL 缓冲液，摇匀，加入200μL 提取液，摇匀，静置10 分钟，加入100μL Sub 试剂，摇匀后移入0.5cm 比色皿，及时放入农药残留测试仪上进行对照测试；
样品测定：
吸取Et 试剂100μL，加入1.5mL 缓冲液，摇匀，加入200μL 待测液，摇匀，静置10 分钟，加入100μLSub 试剂，摇匀后移入0.5cm 比色皿，及时放入农药残留测试仪上进行样品测试。
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| CN102565240A (zh) * | 2011-12-29 | 2012-07-11 | 烟台大学 | 一种对食品中有机氯农药残留检测的样品前处理方法 |
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| CN1096537A (zh) * | 1993-06-18 | 1994-12-21 | 杨卓舒 | 一种果蔬清洗剂 |
| CN1211616A (zh) * | 1997-09-12 | 1999-03-24 | 王中甫 | 瓜果蔬菜残留农药消毒清洗剂 |
| CN103255007A (zh) * | 2012-02-16 | 2013-08-21 | 上海植晶生物科技有限公司 | 农药残留清洗剂 |
| CN103983723B (zh) * | 2014-05-19 | 2015-12-30 | 莱阳恒润食品有限公司 | 水果蔬菜中双胍辛胺残留量检测方法 |
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Non-Patent Citations (3)
| Title |
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| 乙酰胆碱脂酶抑制率法可快速检测米面果蔬中有机磷农药残留;蒲晓亚 等;《食品质量安全与检测》;20080831;第53页第2.1-2.2节 * |
| 有机磷农药对乙酰胆碱酯酶活性的联合抑制作用;颜冬云 等;《农药》;20060131;第45卷(第1期);第32页第1.2-1.3页 * |
| 茶中有机磷及氨基甲酸脂农药残留量的简易检验方法 酶抑制法;中华人民共和国国家质量监督检验检疫总局;《中华人民共和国国家标准GB/T 18625-2002》;20020128;第1-2页第3-5节 * |
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