果冻类样品中非法添加物质2种提取方法比较

Comparative study on 2 extractive methods for the extraction of illegal additives in jelly samples

中文关键词:  果冻类样品  加热处理法  粉碎离心处理法

英文关键词:jelly sample  routine heated method  pulverized centrifugal processed method

中文摘要:

      目的 比较常规加热法和粉碎离心法对果冻类样品中非法添加物质的提取效果。方法 以常见的2种降糖类、4种减肥类和3种利尿类非法添加化学物质为研究对象制备基质加标阳性样, 样品经加热和粉碎离心处理后采用超高效液相色谱串联质谱仪测定, 外标法定量, 以基质效应、回收率和精密度为指标考察2种方法的提取效率。结果 加热处理下样品的回收率为31.27%~135.50%, 精密度为0.75%~16.40%, 经粉碎离心提取处理下的样品中的9种非法添加化学药物回收率为51.60%~116.90%, 精密度为1.63%~10.70%, 粉碎离心处理下样品的基质效应也低于加热处理。结论 相较于加热提取法, 粉碎离心提取法操作简便、结果稳定可靠、灵敏度高, 可用于果冻类胶质样品的样品前处理。

英文摘要:

      Objective To compare the extraction effect of illegal additives in jelly samples by routine heated method and pulverized centrifugal method. Methods Totally 9 illegally additives, including 2 antidiabetic drugs, 4 weight-loss pills and 3 diuretics were used as the research objects to prepare matrix spiked positive samples. After being heated, crushed and centrifuged, the samples were determined by ultra performance liquid chromatography tandem mass spectrometer (UPLC-MS/MS), and quantified by external standard method. The extraction efficiency of the 2 methods was investigated with matrix effect, recovery and precision as indexes. Results Under heat treatment, the recovery rate was 31.27%?135.50% and the precision was 0.75%?16.40%. While, the recovery rate of the 9 illegally additives in the pulverized samples was 51.60%?116.90%, and the precision was 1.63%?10.70%. Besides, the matrix effect under pulverization and centrifugation was lower than that of heat treatment. Conclusion Compared with the heating extraction method, the crushing centrifugal extraction method is easy to operate, and can be used for sample pretreatment of jelly-like samples with more stable, reliable and sensitive results.