液相色谱-质谱联用法测定营养强化粉中烟酰胺的含量

Determination of content of niacinamide in nutritionally fortified powders by liquid chromatography-mass spectrometry

中文关键词:  烟酰胺  液相色谱-质谱联用法  营养强化粉

英文关键词:nicotinamide  liquid chromatography-mass spectrometry  nutritionally fortified powder

中文摘要:

      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, 3 μm); 流速:0.4 mL/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1.5 μg/g, 线性范围为0.0625~0.308 μg/mL(r2=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。

英文摘要:

      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 mL/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/mL (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.