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反相液相色谱法测定蜂蜜中磺胺噻唑残留量

Reverse phase liquid chromatographic determination of sulfathiazole residues in honey.

作者信息

Barry C P, MacEachern G M

出版信息

J Assoc Off Anal Chem. 1983 Jan;66(1):4-7.

PMID:6826511
Abstract

Sulfathiazole residues were extracted from honey by homogenizing samples in acetone, filtering, and then evaporating the acetone under nitrogen at 40 degrees C. The remaining extract was transferred to a separatory funnel with 1N HCl and ethyl ether. An aliquot of the retained acid layer was screened by using the Bratton-Marshall reaction. If the test was positive, the remaining portion was analyzed directly through a mu Bondapak phenyl column monitored by a UV detector at 254 nm. The mobile phase was potassium phosphate monobasic in 10% acetonitrile adjusted to pH 3.0. Time for elution was 13 min. Average recoveries were 78% at the 0.1 ppm spiking level and 68% at the 1.0 ppm level. The minimum detectable amount was 0.06 ppm based on a spiked sample extract.

摘要

通过将蜂蜜样品在丙酮中匀浆、过滤,然后在40℃下用氮气蒸发丙酮来提取磺胺噻唑残留。将剩余提取物转移至装有1N盐酸和乙醚的分液漏斗中。取一部分保留的酸层,采用布拉顿-马歇尔反应进行筛选。如果测试呈阳性,则通过μ Bondapak苯基柱直接分析剩余部分,该柱由254nm的紫外检测器监测。流动相是10%乙腈中的磷酸二氢钾,pH值调至3.0。洗脱时间为13分钟。在0.1ppm加标水平下的平均回收率为78%,在1.0ppm水平下为68%。基于加标样品提取物,最低检测量为0.06ppm。

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