超高效液相色谱-四极杆/轨道阱高分辨质谱法快速筛查功能性保健食品中19种特征性成分

Rapid screening of 19 kinds of characteristic components in functional health food by ultra performance liquid chromatography-quadrupole/orbital trap high resolution mass spectrometry

中文关键词:  功能性保健食品  特征性成分  超高效液相色谱-四极杆/静电场轨道阱高分辨质谱  质谱数据库  定量分析

英文关键词:functional health food  characteristic component  ultra performance liquid chromatography quadrupole/orbitrap trap high resolution mass spectrometry  mass database  quantification

中文摘要:

      目的 建立超高效液相色谱-四极杆/轨道阱高分辨质谱法快速筛查功能性保健食品中19种特征性成分的分析方法。方法 以甲醇为提取液, 样品经超声、高速离心、过滤, 通过XDB-C18色谱柱分离, 以0.1%甲酸溶液(含0.02 mol/L醋酸铵)和甲醇作为流动相梯度洗脱, 选择正负离子实时切换和一级离子/自动触发二级离子扫描模式, 利用保留时间、一级离子和二级离子信息建立质谱数据库, 完成定性分析, 利用一级分子离子峰完成定量测定。结果 19种特征性成分的一级离子质荷比实测值与理论值相对偏差均小于等于8.10×10-6, 19种特征性成分在其相应的线性范围内存在线性关系, 相关系数均大于0.99, 检出限为0.25~1.00 mg/kg, 加标回收率为72.33%~97.93%, 精密度为1.09%~4.86%。结论 该方法抗干扰能力强, 准确度高, 可用于保健食品中19种特征性成分的快速筛查, 同时结合产品标签标识, 鉴别其使用原料的真伪性。

英文摘要:

      Objective To establish a rapid method for screening 19 kinds of characteristic components in functional health food by ultra performance liquid chromatography quadrupole/orbitrap trap high resolution mass spectrometry. Methods Methanol was used as the extraction solvent. After ultrasonic, high-speed centrifugation and filtration, the separation was performed on XDB-C18 column using 0.1% aqueous formic acid (0.02 mol/L ammonium acetate) and methanol as the mobile phase for gradient elution. The real-time switching of positive and negative ions and the primary ion/automatic trigger secondary ion scanning mode were selected, a mass spectrometry database was established using the retention time, primary ion and secondary ion information, so as to complete the qualitative analysis, and complete the quantitative determination using the primary molecular ion peak. Results The relative deviations between the measured mass number of ions of 19 kinds of characteristic components and the theoretical values were less than or equal to 8.10×10?6. The 19 kinds of characteristic components had good linearity within their corresponding linear ranges, and all correlation coefficients were higher than 0.99. The limits of detection were 0.25?1.00 mg/kg, the recoveries were in the range of 72.33%?97.93% with the precision of 1.09%?4.86%. Conclusion The method has strong anti-interference ability and high accuracy and can meet the rapid screening of 19 kinds of characteristic components in functional health food. At the same time, the authenticity of the raw materials can be identified by combining with the product label.