应用GB 5009.89-2016检测乳粉中烟酸和烟酰胺含量实例及探讨

Application and discussion of detection of niacin and nicotinamide in milk powder by GB 5009.89-2016

中文关键词:  高效液相色谱法  乳粉  烟酸  烟酰胺  GB 5009.89-2016

英文关键词:high performance liquid chromatography  milk powder  niacin  nicotinamide  GB 5009.89-2016

中文摘要:

      目的 探讨说明使用GB 5009.89-2016的高效液相色谱法进行实际乳粉中烟酸和烟酰胺含量检测时容易产生误解的细节, 并提出适当建议。方法 样品按照标准方法进行处理与检测, 考察烟酸和烟酰胺的色谱峰形、分离度及响应值; 以连续6次重复进样的相对标准偏差来检验方法的精密度; 以加标回收法来检验方法的准确度。结果 在该方法条件下, 烟酸和烟酰胺的色谱峰分离完全, 响应值高, 峰形尖锐对称; 烟酸和烟酰胺色谱峰的保留时间分别在8.438 min和10.515 min附近, 相对标准偏差分别为0.085%和0.079%; 烟酸的加标回收率为94.4%, 烟酰胺的加标回收率为95.1%。结论 为了保证实验的重复性和结果的准确性, 建议样品前处理过程中的称样量和稀释倍数为确切的数值。在此前提下运用该方法检测乳粉中烟酸和烟酰胺含量精密度高, 结果准确可靠。

英文摘要:

      Objective To discuss misunderstood details that encountered in actual detection work of niacin and nicotinamide in milk powder by high performance liquid chromatography of GB 5009.89-2016, and put forward suggestions. Methods Samples were processed and tested according to standard method. The chromatographic peaks, separation and response values of niacin and nicotinamide were investigated. The precision of the method was tested with a relative standard deviation of 6 replicate injections. Standard recovery experiment was implemented to test the accuracy of the method. Results Under the conditions of this method, niacin and nicotinamide chromatographic peak separation was completely separated, the response was strong and the peak sharp was symmetrical. The retention times of niacin and nicotinamide peaks were near 8.438 min and 10.515 min, and the relative standard deviations were 0.085% and 0.079%, respectively. The standard recoveries of niacin and nicotinamide were 94.4% and 95.1%, respectively. Conclusion In order to ensure the reproducibility of the experiment and the accuracy of the results, it is recommended that the sample amount and dilution factor during the sample pretreatment is the exact values. Under this premise, the method is accurate and reliable in the determination of niacin and nicotinamide in milk powder.