1. 上海市农业科学院林木果树研究所上海市设施园艺技术重点实验室
2. 江苏省中国科学院植物研究所
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李青竹, 张永春, 郑玉红, 等. 超高效液相色谱-四极杆线性离子阱质谱法同时检测石蒜属3种生物碱[J]. 分析测试学报, 2018,37(2):211-216.
Simultaneous Determination of Three Alkaloids in Lycoris spp. by UPLC-QTRAP-MS/MS[J]. 2018,37(2):211-216.
基于超高效液相色谱-串联四极杆/线性离子阱质谱(UPLC-QTRAP-MS/MS),建立了一种同时检测石蒜属植物中加兰他敏(Gal)、力可拉敏(Lycm)和石蒜碱(Lyc)含量的方法。提取液超声波辅助提取离心后,经Waters ACQUITY UPLC BEH C18(150 mm×2.1 mm,1.7 μm)色谱柱,以水溶液(0.1%甲酸)-乙腈为流动相梯度洗脱,流速0.2 mL/min,在正离子扫描下以MRM模式进行分析。结果表明,Gal、Lycm和Lyc在0.5~500 μg/L质量浓度范围内线性关系良好,相关系数达0.999 9~1.000 0,可在6.0 min内得到检测结果,Gal、Lycm和Lyc的保留时间分别为2.86、2.31、1.95 min。3种物质的加标回收率为97.2%~98.6%,相对标准偏差为0.8%~4.3%。应用此方法测得石蒜属12个种的Gal、Lycm和Lyc含量分别在21.98~496.77、0.17~467.21、9.34~4 510.18 μg/g干重之间,3种物质含量在种间差异均较大。
An analytical method based on ultra performance liquid chromatography-quadrupole linear ion trap mass spectrometry(UPLC-QTRAP-MS/MS) was established for the simultaneous determination of galanthamine(Gal),lycoramine(Lycm) and lycorine(Lyc) in Lycoris.After ultrasonic-assisted extraction and centrifugation,the sample was seperated on a Waters ACQUITY UPLC BEH C18 column(150 mm×2.1 mm,1.7 μm) by gradient elution with acetonitrile-water(0.1% formic acid) as mobile phase at a flow rate of 0.2 mL/min.The three target compounds were analyzed in the positive ion multiple reaction monitoring(MRM) mode.Results showed that good linearities for the analytes were obtained in the concentration range of 0.5-500 μg/L with their correlation coefficients of 0.999 9-1.000 0 within 6 mins,and the retention times for Gal,Lycm and Lyc were 2.86 min,2.31 min and 1.95 min,respectively.The average recoveries were between 97.2%-98.6% with relative standard deviations of 0.8%-4.3%. The contents of Gal,Lycm and Lyc in 12 Lycoris species were determined to be 21.98-496.77 μg/g,0.17-467.21 μg/g and 9.34-4 510.18 μg/g by dry weight,respectively.Large differences were observed among species.This method was sensitive and accurate,and could provide a reliable and effective approach for the accumulation detection and metabolic regulation of alkaloids in Lycoris.
石蒜超高效液相色谱-串联四极杆/线性离子阱质谱加兰他敏力可拉敏石蒜碱
LycorisUPLC-QTRAP-MS/MSgalanthaminelycoraminelycorine
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