Simultaneous Cleanup Method for Multi Pesticide Residue Analysis by GC and HPLC
Simultaneous Cleanup Method for Multi Pesticide Residue Analysis by GC and HPLC
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通过 GC 和 HPLC 进行多种农药残留分析的同时净化方法
DOI：
10.3358/shokueishi.39.4_241
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发表时间：
1998
期刊：
影响因子：
--
通讯作者：
Fumitaka Tanaka
中科院分区：
文献类型：
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作者：
Y. Shibata;Mayumi Oyama;H. Sato;Kazuko Nakao;M. Tsuda;Masanori Sonoda;Fumitaka Tanaka
建立了气相色谱-高效液相色谱同时净化检测农产品中农药残留的方法，考察了120种农药在硬凝胶型GPC柱和ENVI™-Carb/LC-NH 2微型柱上的洗脱模式。大部分农药在55- 160 mL的GPC洗脱液中用30%丙酮-环己烷（v/v）洗脱，在0- 20 mL的微型柱洗脱液中用25%甲苯-乙腈（v/v）洗脱。结果表明，这两种净化方法对大多数农药都适用。萃取物用饱和硫酸铵-乙酸乙酯分配。将提取物脱水，真空蒸发，溶解在GPC移动的相中，并通过GPC净化。将农药的洗脱部分在真空中蒸发并溶解在丙酮中。在微型柱上净化丙酮溶液的等分试样。真空蒸发沉淀物并溶于丙酮或乙腈中。样品用气相色谱法或高效液相色谱法测定。对6种农产品中的120种农药进行了分析，其中110种农药的回收率较好，可满足GC和HPLC农药残留检测的要求。
A simultaneous cleanup method for the determination of pesticide residues in agricultural products by GC and HPLC was developed.The elution patterns of 120 pesticides from a hard gel-type GPC column and an ENVI™-Carb/LC-NH2 mini-column were examined. Most of the pesticides were eluted in the 55-160mL fraction from GPC with 30% acetone-cyclohexane (v/v) and in the 0-20mL fraction from the mini-column with 25% toluene-acetonitrile (v/v). The results showed that these two cleanup methods were applicable for most of the pesticides.A sample was extracted with acetone and filtered. The extract was partitioned with saturated ammonium sulfate-ethyl acetate. The extract was dehydrated, evaporated in vacuo, dissolved in the GPC mobile phase and cleaned up by GPC. The eluate fraction of pesticides was evaporated in vacuo and dissolved in acetone. An aliquot of the acetone solution was cleaned up on a mini-column. The eluate was evaporated in vacuo and dissolved in acetone or acetonitrile. The sample was determined with GC or HPLC. The additional mini-column cleanup was especially effective for HPLC analysis.Approximately 110 out of 120 pesticides spiked into 6 kinds of agricultural products gave good recoveries with combined cleanup using GPC and the mini-column, which is considered to be satisfactory for pesticide residue monitoring by GC and HPLC.