首页> 中文期刊> 《分析测试学报》 >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

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

         

摘要

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.%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 C1s(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0.9999~1.0000,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.

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