超高效液相色谱-串联质谱法快速测定保健食品中大豆异黄酮含量

建立保健食品中6种大豆异黄酮的超高效液相色谱串联质谱(UPLC-MS/MS)同时检测方法。样品中大豆异黄酮采用80%甲醇超声提取、Florisil固相萃取柱净化,C₁₈色谱柱分离,以0.1%甲酸水溶液和乙腈为流动相,流速0.3 mL/min,柱温30 ℃,质谱正离子多反应监测(MRM)模式进行检测。结果表明,大豆苷、大豆黄苷、染料木苷、大豆素、大豆黄素以及染料木素在各自浓度范围内线性关系良好;大豆黄苷、大豆黄素检出限均为10 μg/kg;大豆苷、染料木苷检出限均为20 μg/kg;大豆素、染料木素检出限均为30 μg/kg,加标回收率为81.8%~98.4%,相对标准偏差为1.8%~6.7%。所建立的超高效液相色谱串联质谱是一种高灵敏度、高准确度的测定方法,对保健食品中大豆异黄酮的质量控制提供了参考依据,具有一定的理论意义和应用价值。

Rapid Determination of Isoflavones Content of Soybean in Health Foods by UPLC-tandem Mass Spectrometry

A method based on ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS /MS) had been developed for simultaneous determination of 6 kinds of soybean isoflavones in health foods.The soybean isoflavones were ultrasonic extracted from contents of soft capsule with 80% methanol,purified by Florisil cartridge and separated by C18 chromatographic column.0.1% formic acid aqueous solution and acetonitrile were used as mobile phase with the flow rate of 0.3 mL/min,the column temperature was 30 ℃,and the positive ion mode with multiple reaction monitoring( MRM) was used to detect soybean isoflavones.Experiments results showed that daidzin,glycitin,genistin,daidzein,glycitein and genistein were linear in their respective concentration range.The limits of detection were 10 μg /kg for glycitin and glycitein,20 μg /kg for daidzin and genistin and 30 μg /kg for daidzein,genistein,respectively.The recoveries ranged from 81.8% to 98.4% with the relative standards deviations of 1.8%~ 6.7%.The results provided a technical reference for quality control and effective utilization of soybean isoflavones in health food,and had certain theoretical significance and application value.