高效液相色谱-串联三重四极杆飞行时间质谱法鉴别五味子中木脂素成分

建立高效液相色谱-串联三重四极杆飞行时间质谱结合QuEChERS前处理技术对五味子中木脂素成分进行快速筛查测定的方法。优化QuEChERS前处理条件，采用Xbridge BEH C18色谱柱分离，梯度洗脱，数据依存获取高分辨质谱检测模式，依据目标物的一级母离子的精确质量数、同位素丰度比二级离子的精确质量数和色谱保留时间等信息定性定量分析五味子醇甲五味子甲素中木脂素成分。结果表明：3?个特征木脂素化合物检测限低（0.3～1.5?μg/L），线性关系良好（R2≥0.999?6）；同时利用木脂素类化合物XIClists表可快速筛查鉴定样品中木脂素分布情况。

Identification of Lignanoids in Schisandra chinensis Fruits by High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

An analytical method using quick, easy, cheap, effective, rugged and safe (QuEChERS) pretreatment combined with high performance liquid chromatography-quadrupole-time of flight mass spectrometry (HPLC-Q-TOF-MS) was established for the quick screening of lignanoids in Schisandra chinensis. Sample pretreatment conditions were optimized. Chromatographic separation was accomplished on an Xbridge BEH C18 column with gradient elution. The mass spectrum was acquired by information dependent acquisition mass spectrometry (IDA-MS). The qualitative and quantitative analyses were based on the accurate masses of parent ions and isotopic patterns, and the accurate masses of fragment ions as well as a priori known retention times. The results showed that the limits of detection (LODs) for the three standards were within the range of 0.3–1.5 μg/L, and calibration curves offered satisfactory linearity (R2 ≥ 0.999 6) in a wide linear range. Lignanoids in S. chinensis samples could be quickly identified by searching in the high-resolution mass spectral library XIClists developed in this study.