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以玛咖中玛咖酰胺为研究对象,研究了玛咖酰胺特征紫外吸收、红外光谱和质谱断裂方式,建立了快速测定玛咖中玛咖酰胺的超高效液相色谱-串联质谱方法。玛咖样品经石油醚-超声辅助提取后,采用ZORBAX C18色谱柱分离,用乙腈-1 mmol/L乙酸铵水溶液(含0.1%甲酸)作为流动相进行梯度洗脱,正离子多反应监测模式。结果表明,玛咖酰胺在0.01~10.0μg/L的含量范围内具有较好的线性关系,检出限为5.0 ng/kg,定量限为20 ng/kg。当加标量为0.02,0.1和0.2μg/kg时,平均回收率为93.5%~116.7%,相对标准偏差为6.3%~11%。方法能够满足玛咖中玛咖酰胺分析测定的要求。
Taking Macahama maca as the research object, the characteristics of Macaamide by ultraviolet absorption, infrared spectrum and mass spectrometry were studied, and the rapid determination of Macaramic acid in Maca by ultra performance liquid chromatography-tandem mass spectrometry was established. Maca samples were extracted by petroleum ether-ultrasound and separated on a ZORBAX C18 column. The mobile phase was eluted with acetonitrile-1 mmol / L ammonium acetate solution (containing 0.1% formic acid). The calibration curve was positive. The results showed that there was a good linear relationship between the concentration of mannamide and 0.01 ~ 10.0μg / L with the detection limit of 5.0 ng / kg and the limit of quantification of 20 ng / kg. The average recovery was 93.5% ~ 116.7% with the relative standard deviations of 6.3% ~ 11% at 0.02, 0.1 and 0.2 μg / kg. The method meets the requirements of the maca-amicacamide assay.