Greenberg R S
Ministry of Agriculture, Plant Protection Department, Bet-Dagan, Israel.
J Assoc Off Anal Chem. 1987 Sep-Oct;70(5):870-4.
A gas chromatographic method is described for determining residues of mecarbam and 3 of its metabolites, mecarboxon, diethoate, and diethoxon, in cottonseeds. For mecarbam analysis, following Soxhlet extraction with chloroform (after blending), the oily extract is partitioned with propylene carbonate and cleaned up on a silica gel column. Metabolites are extracted by the same method, followed by cleanup of mecarboxon on a silica gel column or diethoxon on an alumina column; cleanup of diethoate can be performed on either column. All 4 compounds are determined using a flame photometric detector equipped with a phosphorus filter. Average recoveries for cottonseed samples fortified with 0.03-1.0 ppm mecarbam ranged from 80 to 88%. Average recoveries were 81-88% for mecarboxon and 90-92% for diethoate (alumina column) and diethoxon from samples fortified with 0.05-1.0 ppm. Average recovery of diethoate from samples cleaned up on the silica gel column were 84-88% in the range of 0.05-0.2 ppm. Values obtained for mecarbam residues in field-treated samples are also presented.
描述了一种气相色谱法，用于测定棉籽中甲萘威及其3种代谢物甲羧威、二嗪磷和二嗪农的残留量。对于甲萘威分析，用氯仿进行索氏提取（混合后），将油性提取物用碳酸丙烯酯进行分配，然后在硅胶柱上净化。代谢物采用相同方法提取，随后甲羧威在硅胶柱上净化，二嗪农在氧化铝柱上净化；二嗪磷的净化可在任一柱上进行。所有4种化合物均使用配备磷滤光片的火焰光度检测器进行测定。添加0.03 - 1.0 ppm甲萘威的棉籽样品的平均回收率为80%至88%。添加0.05 - 1.0 ppm的样品中甲羧威的平均回收率为81%至88%，二嗪磷（氧化铝柱）和二嗪农的平均回收率为90%至92%。在0.05 - 0.2 ppm范围内，在硅胶柱上净化的样品中二嗪磷的平均回收率为84%至88%。还给出了田间处理样品中甲萘威残留量的测定值。
