LC-MS/MS法测定桑枝中的核苷类成分  

Determination of nucleosides in mulberry branches by LC-MS/MS

作　　者：黄小兰 何旭峰 周浓 伍蓉 冉华康 张椿翊 HUANG Xiaolan;HE Xufeng;ZHOU Nong;WU Rong;RAN Huakang;ZHANG Chunyi(Chongqing Wanzhou Food and Drug Inspection Institute,Chongqing,404100 P.R.China;College of Biology and Food Engineering,Chongqing Three Gorges University,Chongqing,404100 P.R.China)

机构地区：[1]重庆市万州食品药品检验所,重庆万州404100 [2]重庆三峡学院生物与食品工程学院,重庆万州404120

出　　处：《华西药学杂志》2024年第2期179-184,共6页West China Journal of Pharmaceutical Sciences

基　　金：重庆市教育委员会科学研究基金项目(KJQN201801210)。

摘　　要：目的测定并分析不同产地、种类桑枝中的10种核苷类成分,为桑枝的质量评价、开发利用提供基础。方法桑枝样品经纯水超声提取,以甲醇-乙酸铵溶液为流动相,在色谱柱(150 mm×4.6 mm,3.5μm)上梯度洗脱,采用LC-MS/MS法在正离子模式下测定,用SPSS 20.0统计软件对结果进行方差分析、相关性分析、主成分分析和聚类分析。结果18批次桑枝中的核苷总含量为0.4115~2.3384 mg·g^(-1),不同产地及种类的桑枝中均以鸟苷、腺苷、胞苷(0.5401、0.3284、0.2690 mg·g^(-1))的含量较高,含量最低的为次黄嘌呤(1.54μg·g^(-1))。相关性分析显示:核苷成分间存在18组极显著正相关,9组显著正相关关系,表明核苷在积累过程中相互促进。主成分分析显示:巴南区安澜镇的鸡桑(S4)综合得分最高,其次为南岸区黄桷垭镇的鸡桑(S8)、北碚区天生街道鸡桑(S13)、奉节新民镇的鸡桑(S14);聚类分析显示:巴南区安澜镇的鸡桑(S4)为Ⅰ类,南岸区黄桷垭镇的鸡桑(S8)为Ⅱ类,其余16批桑枝样品为Ⅲ类。结论不同产地及种类桑枝中均含有较高的核苷类成分,整体来说鸡桑的品质优于华桑和桑,具有开发利用价值。OBJECTIVE To determine and analyze the 10 nucleosides in mulberry branches of different varieties from different origins.METHODS The mulberry branch samples were extracted by ultrasonic extraction in pure water,and then gradient elution was performed on column(150 mm×4.6 mm,3.5μm)with methanol-ammonium acetate solution as mobile phase.The samples were then determined by LC-MS/MS technique in positive ion mode.The results were analyzed by variance analysis,correlation analysis,principal component analysis and cluster analysis using SPSS 20.O statistical software.RESULTS 10 nucleosides were detected in 18 batches of mulberry branches,with significant dfferences in total contents ranging from 0.4115 mg·g^(-1)to 2.3384 mg·g^(-1).The content of guanosine(0.5401 mg·g^(-1)),adenosine(0.3284 mg·g^(-1))and cytidine(0.2690 mg·g^(-1))was higher in mulberry branches from different producing areas and species,and the lowest content was hypoxanthine(1.54μg·g^(-1)).There were 18 groups of extremely significant positive correlation among nucleosides,and 9 groups of significant positive correlation,indicating that nucleosides promote each other in the accumulation process.The results of principal component analysis showed that the comprehensive score of chicken mulberry(S4)in Anlan town,Banan District was the highest,followed by Chicken mulberry(S8)in Huangjueya town,Beibei District(S13)and Chicken mulberry(S14)in Fengjie Xinmin town.The cluster analysis results showed that the chicken mulberry(S4)from Bolan town,Banan District was in the same category,the chicken mulberry(S8)from Huangjueya Town,Nanan District,and the other 16 batches of mulberry branch samples were in the same category.CONCLUSION There are high levels of nucleosides in mulberry branches of different varieties from different origin,and the quality of chicken mulberry was better than that of Huasang and mulberry,which can be developed and utilized.

关 键 词：桑枝 核苷 液相色谱-串联质谱法 含量测定 相关性分析 主成分分析 聚类分析 质量评价 

分 类 号：R917[医药卫生—药物分析学]