桑枝中1-脱氧野尻霉素的定性定量分析  

Qualitative and quantitative analysis of 1-deoxynojirimycin in Ramulus mori

作　　者：孙莲[1] 殷超 杜申道 SUN Lian;YIN Chao;DU Shendao(Department of Chemistry,Xinjiang Medical University,Urumqi 830011,China)

机构地区：[1]新疆医科大学化学教研室,乌鲁木齐830011

出　　处：《西北药学杂志》2020年第4期489-494,共6页Northwest Pharmaceutical Journal

基　　金：细胞生物学国家重点实验室课题项目(编号:2018-1-20);新疆维吾尔自治区“十三五”重点学科建设经费资助项目(新教研[2016]7号)。

摘　　要：目的建立桑枝中1-脱氧野尻霉素(1-DNJ)的定性、定量分析方法。方法采用TLC法定性鉴定桑枝中的1-DNJ,并对测定条件进行优化。采用HPLC法测定1-DNJ的含量,以YMC-C18柱(250 mm×4.6 mm,5μm)为色谱柱;以醋酸(A)-1 mL·min^-1甲醇(B)进行梯度洗脱;柱温:25℃;流速:1.0 mL·min^-1;检测波长:254 nm。结果在硅胶G板上,以冰醋酸-正丁醇-水(24∶90∶24)为展开剂,在室温条件下展开,邻-联甲苯胺显色,可见光检视时1-DNJ的分离度良好,斑点圆整、清晰。1-DNJ的线性范围为10.03~100.28μg·mL^-1,r=0.999 5,平均回收率为99.8%,RSD值为1.1%。不同产地桑枝中1-DNJ的含量在50.37~179.52μg·g^-1范围内。结论该方法简单易行,结果可靠,可用于桑枝的质量控制与评价。Objective To establish qualitative and quantitative methods for the evaluation of Ramulus mori.Methods The determination conditions of TLC for qualitative determination of 1-deoxynojirimycin in Ramulus mori were optimized.The content of 1-deoxynojirimycin was determined by HPLC.The chormatograhic separation was performed on YMC-C18 column(250 mm×4.6 mm,5 μm);the column temperature was maintained at 25 ℃;gradient elution was adapted by using acetic acid and methanol;the flow rate was 1.0 mL·min^-1;the UV detection wavelength was 254 nm.Results 1-deoxynojirimycin in Ramulus mori from silica gel G were detected and separated successfully with acid-n-butanol-water(24∶90∶24) as developer and 3,3′-dimethy lbiphenyl-4,4′-diamine solution as chromogenic reagent at room temperature.The 1-deoxynojirimycin in Ramulus mori was colored clearly and the spot of 1-deoxynojirimycin was round,clear and well separated when observed under visible light.1-deoxynojirimycin showed good linearity in the ranges of 10.03-100.28 μg·mL^-1(r=0.999 5).The recovery was 99.8% with RSD 1.1%.And the contents of 1-deoxynojirimycin in Ramulus mori from different area were 50.37-179.52 μg·g^-1.Conclusion The method is simple and has satisfactory efficacy.It could be used for the evaluation and quality control of Ramulus mori.

关 键 词：桑枝 1-脱氧野尻霉素 TLC法 HPLC法 

分 类 号：R284[医药卫生—中药学]