College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, China.
Zhejiang Institute for Food and Drug Control, Hangzhou, China.
J Sep Sci. 2017 Dec;40(24):4857-4864. doi: 10.1002/jssc.201700626. Epub 2017 Dec 1.
A novel method based on direct analysis in real time integrated with mass spectrometry was established and applied into rapid determination of ginkgolic acids in Ginkgo biloba kernels and leaves. Instrument parameter settings were optimized to obtain the sensitive and accurate determination of ginkgolic acids. At the sample introduction speed of 0.2 mm/s, high intensity of [M-H] ions for ginkgolic acids were observed in the negative ion mode by utilization of high-purity helium gas at 450°C. Two microliters of methanol extract of G. biloba kernels or leaves dropped on the surface of Quick-Strip module was analyzed after solvent evaporated to dryness. A series of standard solutions of ginkgolic acid 13:0 in the range of 2-50 mg/L were analyzed with a correlation coefficient r = 0.9981 and relative standard deviation (n = 5) from 12.5 to 13.7%. The limit of detection was 0.5 mg/L. The results of direct analysis in real time-mass spectrometry were in agreement with those observed by thermochemolysis gas chromatography. The proposed method demonstrated significant potential in the application of the high-throughput screening and rapid analysis for ginkgolic acids in dietary supplements.
建立了一种基于实时直接分析与质谱联用的新方法,并将其应用于快速测定银杏果仁及叶片中的白果酸。优化了仪器参数设置,以实现对白果酸的灵敏准确测定。在样品导入速度为 0.2mm/s 时,通过在 450°C 下使用高纯氦气,在负离子模式下观察到白果酸的[M-H]离子强度较高。将 2 微升银杏果仁或叶片的甲醇提取物滴在 Quick-Strip 模块表面,待溶剂蒸发至干燥后进行分析。在 2-50mg/L 范围内,对一系列 13:0 白果酸标准溶液进行分析,相关系数 r=0.9981,相对标准偏差(n=5)为 12.5-13.7%。检测限为 0.5mg/L。实时直接分析-质谱的结果与热化学裂解气相色谱的结果一致。该方法在膳食补充剂中白果酸的高通量筛选和快速分析方面具有很大的应用潜力。