出来混迟早要还的
第3楼2013/01/02
因为是测土壤中的残留量，所以这个方法很麻烦--强酸加有机溶剂萃取后，polymer SPE净化，浓缩衍生后，再上$$lcMSMS. 试过前两步后，直接浓缩上$$lcMSMS，C18上基质效应还挺强，但检测限到0.01ppm没有问题。
有人有下面这个的全文吗，似乎水果蔬菜上的基质效应不高。
J AOAC Int. 2012 Mar-Apr;95(2):554-9.
Simultaneous determination of aminopyralid, clopyralid, and picloram residues in vegetables and fruits using ultra-performance liquid chromatography/tandem mass spectrometry.
Tian Y, Liu X, Dong F, Xu J, Lu C, Kong Z, Wang Y, Zheng Y.
Source
Chinese Academy of Agricultural Sciences, Institute of Plant Protection, Ministry of Agriculture, Key Laboratory of Pesticide Chemistry and Application, Beijing 100193, People's Republic of China.
Abstract
A sensitive and effective method for the simultaneous quantitative determination of aminopyralid, clopyralid, and picloram in vegetables (eggplant, cucumber, and tomato) and fruits (apple and grape) was developed and validated using ultra-performance $$lc coupled with MS/MS. The three herbicides were successfully separated and independently confirmed in a single run. Different extraction and cleanup methods were used to optimize the pretreatment processes of the residue analysis method. The final method is straightforward and involves extraction with 1% formic acid-acetonitrile, and no complicated cleanup process is needed. Determination of the compounds was achieved within 3.0 min. Respective average recoveries using this method at four concentration levels (0.05, 0.1, 0.5, and 1.0 mg/kg) ranged from 66.5 to 109.4%, with RSDs in the range of 1.1-19.7% (n = 5) for all analytes. The LODs were below 0.010 mg/kg, and the LOQs did not exceed 0.036 mg/kg, which were lower than the maximum residue limits (MRLs) of 0.5-5.0 mg/kg clopyralid in vegetables and fruits samples, as established by the European Union. This study provides a theoretical basis for China to develop MRLs and an analytical method for aminopyralid, clopyralid, and picloram in vegetables and fruits.
雾非雾
第10楼2013/02/07
应助达人2013-1-23 9:44:00 来源：世界农化网
陶氏益农除草剂氯氨吡啶酸（aminopyralid）原药及其水剂在中国取得临时登记。
近日，陶氏益农除草剂氯氨吡啶酸（aminopyralid）原药及其水剂在中国取得临时登记。氯氨吡啶酸为陶氏益农公司开发的卤代吡啶类除草剂。2005年在加拿大和美国以Milestone商品名首次登记用于牧场，而后，陶氏益农开发出该除草剂与其它谷物除草剂复配的新用途，向世界各地推出多达30个复配产品，还被进一步拓展用于油菜、玉米和油棕榈等作物。
然而，陶氏益农除草剂氯氨吡啶酸近几年也是风波不断。2008年，由于氯氨吡啶酸除草剂能持续存留在农田堆肥中，对后续的作物产生大范围的损害。英国农业管理部门对这个产品发布了使用禁令。直到2009年，陶氏同意限制使用范围之后，才重新放行这个产品。为防后茬作物受损，美国环保署对陶氏益农氯氨吡啶酸类除草剂实施强制性附加限制，禁止使用过该农药后的干草在极易对作物产生损害的地区进行销售。预计将大大减少这个除草剂的使用范围。2011年年初，氯氨吡啶酸在澳大利亚五年知识产权保护到期。
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