HPLC法检测乳制品中糖精钠样品前处理方法研究  

Progress on sample preparation techniques for analysis of Sodium saccharin in milk by High Performance Liiquid Chromatography( HPLC)

作　　者：李伟昊[1] 丁国涛 杨国兴[1] 靳増军 连莹莹[1] 韩永红[1] 

机构地区：[1]邯郸市疾病预防控制中心,河北056008

出　　处：《医学动物防制》2018年第1期37-38,41,共3页Journal of Medical Pest Control

基　　金：河北省重点研发计划项目(17275505D)

摘　　要：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 Establish a sample preparation method for analysis of Sodium saccharin in milk by High Performance Liquid Chromatography（ HPLC）. Methods Four versions of milk sample preparation method for determination of Sodium saccharin by HPLC were been compared and improved. Results The precision of potassium ferrocyanide-zinc acetate was 1. 397%,the recovery rate was 95. 40% ~ 102. 05%. The precision of lead acetate-potassium oxalate potassium phosphate was 1. 868%,the recovery rate was 91. 05% ~ 98. 93%. The precision of absolute ethanol method was 1. 857%,the recovery rate was 107. 03% ~110. 60%. The precision of trichloroacetic acid method was 2. 257%,the recovery rate was 78. 90% ~ 85. 30%. By optimizing the centrifugal speed to improve the centrifugal effect,shorten the pretreatment time,and did not appear excessive centrifugal recovery rate caused by the phenomenon. Conclusion Through compared the RSD and recovery rate of four preparation methods,a convenient,fast,accurate method was established.

关 键 词：高效液相色谱 糖精钠 乳制品 样品处理 

分 类 号：R155.5[医药卫生—营养与食品卫生学]