利用超高效液相色谱-三重四级杆串联质谱联用技术(UPLC MS/MS),对黑豆皮中花青苷类物质进行定性分析。黑豆皮经石油醚索氏提取和6%甲酸水溶液回流提取,取上清液,超滤后用UPLC MS/MS、ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱,以6%甲酸和乙腈为流动相,进行梯度洗脱,在电喷雾(ESI)正离子模式下,用MRM模式监测。在黑豆皮中检测出矢车菊素类、芍药素类、天竺葵素类、锦葵素类、矮牵牛素类和飞燕草素类这6类共15种花青苷类物质,矢车菊素-3,5-双葡萄糖苷、矢车菊素-3-芸香糖苷、芍药素-3,5-双葡萄糖苷、芍药素-3-半乳糖苷、锦葵素-3-半乳糖苷、锦葵素-3-葡萄糖苷、矮牵牛素-3-半乳糖苷、矮牵牛素这8种花青苷在黑豆皮花青苷类物质研究中未见报道。通过对黑豆皮花青苷类物质的分析,建立了UPLC MS/MS检测黑豆皮中花青苷类物质方法,该方法具有操作简便、准确、快速、选择性强的特点。

A determination method of ultra performance liquid chromatography-triple quadrupole mass spectrometry( UPLC MS /MS) was developed for qualitative analyzing of anthocyanins. After black soybean was extracted through petroleum ether,the reflux was extracted by 6% formic acid,the supernatant was then ultrafiltrated. The analysis was carried out by ACQUITY UPLC BEH C18column( 2. 1 mm × 50 mm,1. 7 μm) as the chromatographic column,6% formic acid and acetonitrile as the mobile phase gradient elution. In electrospray ionization( ESI) positive ion mode,electrospray positive ion multiple reaction monitoring( MRM) was used for monitoring. Six kinds anthocyanins including cyanidins,peonidins,petunidins,delphinidins,pelargonidins and malvidins,totally 15 anthocyanins were detected. Among these 15 anthocyanins,8 compounds,cyanidin-3,5-diglucoside,cyanidin-3- rutinose,peonidin-3,5-diglucoside,peonidin-3-galactoside,malvidin-3-galactoside,malvidin-3-glucoside,petunidin-3-galactoside and petunidin have not been reported in any studies of anthocyanins in black soybean. UPLC MS /MS was a successful method because it is simple,accurate,rapid and highly selective.