Barry C P, MacEachern G M
J Assoc Off Anal Chem. 1983 Jan;66(1):4-7.
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.
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。