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目的建立乳制品中糖精钠检测的前处理方法。方法比较4种前处理方法亚铁氰化钾-乙酸锌法、乙酸铅-草酸钾磷酸氢二钾法、无水乙醇法、三氯乙酸法对高效液相色谱法检测糖精钠的影响,并对方法进行优化。结果亚铁氰化钾-乙酸锌法精密度1.397%,回收率95.40%~102.05%;乙酸铅-草酸钾磷酸氢二钾法精密度1.868%,回收率91.05%~98.93%;无水乙醇法精密度1.857%,回收率107.03%~110.60%;三氯乙酸法精密度2.257%,回收率78.90%~85.30%。通过优化离心速度提高了离心效果,缩短了前处理时间,且未出现过度离心造成的回收率降低的现象。结论经过试验比较4种前处理方法的精密度、回收率,得出了适用于乳制品中糖精钠前处理的简便、快捷、准确的前处理方法。
Objective To establish a pretreatment method for the determination of sodium saccharin in dairy products. Methods The effects of four pretreatment methods, such as potassium ferrocyanide-zinc acetate method, lead acetate-potassium oxalate dipotassium hydrogen phosphate method, anhydrous ethanol method and trichloroacetic acid method, on the determination of sodium saccharin by HPLC Method optimization. Results The precision of potassium ferrocyanide-zinc acetate method was 1.397% and the recovery was 95.40% -102.05%. The lead acetate-potassium oxalate dipotassium hydrogen phosphate method was 1.868% with the recovery of 91.05% -98.93%. The absolute ethanol method The precision was 1.857% and the recovery rate was 107.03% ~ 110.60%. The precision of trichloroacetic acid was 2.257% and the recovery was 78.90% ~ 85.30%. By optimizing the centrifugation speed, the centrifugal effect is improved, the pre-treatment time is shortened, and the recovery rate caused by over-centrifugation is not reduced. Conclusions After comparing the precision and recovery rate of the four pretreatment methods, a simple, rapid and accurate pretreatment method for the pretreatment of saccharin sodium in dairy products was obtained.