Arenas R V, Johnson N A
Merck & Co., Inc., Merck Research Laboratories, Three Bridges, NJ 08887-0450, USA.
J AOAC Int. 1995 May-Jun;78(3):642-6.
A novel liquid chromatographic multiresidue method has been developed for quantitation of thiabendazole (TBZ), the metabolite 5-hydroxythiabendazole (5-OH-TBZ), and the sulfate conjugate of 5-hydroxythiabendazole (5-HSO4-TBZ) in raw cow's milk. The 5-HSO4-TBZ is hydrolyzed quantitatively under acidic conditions to 5-OH-TBZ. TBZ and 5-OH-TBZ are extracted from milk at pH 8.0 with ethyl acetate followed by cleanup of the extract on a cation-exchange solid-phase extraction column. Analytes are quantitated by liquid chromatography with a cation-exchange stationary phase and fluorescence detection. Recoveries from raw cow's milk samples fortified with TBZ and 5-OH-TBZ or TBZ and 5-HSO4-TBZ at 0.05 to 2 ppm ranged from 87 to 103% for TBZ, 98-109% for 5-OH-TBZ, and 96-115% for 5-HSO4-TBZ (quantitated as 5-OH-TBZ). The assay provides a simple, rapid, and sensitive multiresidue method for monitoring total residues of TBZ, 5-OH-TBZ, and 5-HSO4-TBZ in milk.
已开发出一种新型液相色谱多残留方法，用于定量测定生牛奶中的噻苯达唑（TBZ）、代谢物5-羟基噻苯达唑（5-OH-TBZ）以及5-羟基噻苯达唑的硫酸酯共轭物（5-HSO4-TBZ）。5-HSO4-TBZ在酸性条件下定量水解为5-OH-TBZ。TBZ和5-OH-TBZ在pH 8.0时用乙酸乙酯从牛奶中萃取，随后在阳离子交换固相萃取柱上对萃取物进行净化。通过使用阳离子交换固定相和荧光检测的液相色谱法定量分析物。在生牛奶样品中添加0.05至2 ppm的TBZ和5-OH-TBZ或TBZ和5-HSO4-TBZ后，TBZ的回收率为87%至103%，5-OH-TBZ为98%至109%，5-HSO4-TBZ（以5-OH-TBZ定量）为96%至115%。该分析方法为监测牛奶中TBZ、5-OH-TBZ和5-HSO4-TBZ的总残留量提供了一种简单、快速且灵敏的多残留方法。
