摘要
目的在国标GB/T 5009.197-2003基础上,建立一种液相色谱-质谱联用法(liquid chromatographymass spectrometry,LC-MS)测定营养强化粉中烟酰胺含量的方法。方法样品经过0.1%甲酸水(含20%甲醇)提取,超声、定容后离心等处理后过滤上机待测。仪器条件为:色谱柱C18(10 cm×4.6 mm,3μm);流速:0.4 m L/min;流动相:水相:乙腈=50:50(V:V);离子峰为(m/z 121.1);选择子离子m/z 80.1和m/z 71.9分别作为定量离子和定性离子。结果该方法中烟酰胺的检出限为1.5μg/g,线性范围为0.0625~0.308μg/m L(r^2=0.9993)。加标平均回收率为96.05%~101.47%,相对标准偏差(relative standard deviation,RSD)为0.4%~1.7%(n=3)。结论本研究建立的方法准确性高,不受样品中杂质峰的影响,同时操作简单、快速,适用于营养强化粉中烟酰胺的测定。
Objective To establish a method for determination of content of niacinamide in nutritionally fortified powders by liquid chromatography-mass spectrometry（LC-MS）, based on the method of GB/T 5009.197-2003. Methods The samples were extracted by 0.1% formate water（containing 20% methanol）. After ultrasonic, centrifugation and other treatment, the filter was tested. The conditions of the instrument were as follows： C18（10 cm×4.6 mm, 3 μm） was used as chromatographic column, flow rate was 0.4 m L/min, the aqueous phase： acetonitrile =50：50（V：V） was used as liquid phase, the ion peak was（m/z 121.1）, and selected subions m/z 80.1 and m/z 71.9 were used as quantitative ions and qualitative ions, respectively. Results The limit of detection of niacinamide was 1.5 μg/g, and the linear range was 0.0625-0.308 g/m L（r2=0.9993）. The average recoveries were 96.05%-101.47% with the relative standard deviations（RSDs） of 0.4%-1.7%（n=3）. Conclusion The established method is accurate, independent of impurity peak, simple and fast, which is suitable for determination of niacinamide in nutritional fortified powder.
作者
蔡伟江
陈珊珊
陈彩云
林丽
梁洁仪
CAI Wei-Jiang;CHEN Shan-Shan;CHEN Cai-Yun;LIN Li;LIANG Jie-Yi(By-Health Co., Ltd., Zhuhai 519040, China)
出处
《食品安全质量检测学报》
CAS
2018年第7期1649-1653,共5页
Journal of Food Safety and Quality
关键词
烟酰胺
液相色谱-质谱联用法
营养强化粉
nicotinamide
liquid chromatography-mass spectrometry
nutritionally fortified powder
