摘要
目的建立不同产地大枣药材的指纹图谱和质量分数测定的UPLC法。方法选择15批全国不同产地的大枣药材,采用UPLC法建立大枣药材指纹图谱,色谱条件:色谱柱为Waters HSS T3柱(150 mm×2.1 mm,1.6μm),流动相为0.1%磷酸-乙腈(梯度洗脱),流速为0.25 mL/min,柱温为30℃,波长为254 nm;采用UPLC法测定大枣药材中环磷腺苷的质量分数,色谱条件:色谱柱为Waters BEH C18柱(100 mm×2.1 mm,1.7μm),流动相为甲醇-0.05 mol/L KH2PO4溶液(体积比8∶92),流速为0.4 mL/min,柱温为30℃,波长为259 nm。结果指纹图谱研究确定了14个共有特征峰,各特征峰分离度良好,并指认了鸟苷、环磷腺苷、5-羟甲基糠醛和芦丁4个已知化合物;15批不同产地大枣药材中环磷腺苷的质量分数范围为101~441μg/g,不同产地间的差异不大,山西省、河南省、甘肃省的较高,山东省和河北省的较低。结论建立的不同产地大枣药材的指纹图谱和含量测定的方法稳定可重复,满足方法学考察要求,可作为大枣药材质量控制方法。
Objective To establish UPLC fingerprints and determination method of Ziziphus jujube from different habitats.Methods 15 batches of jujube products were selected from different habitats.UPLC was used to establish fingerprints of Ziziphus jujube.Waters HSS T3(150 mm×2.1 mm,1.6μm)column was used with 0.1%phosphoric acid and acetonitrile as mobile phase(gradient elution)at the flow rate of 0.25 mL/min.The column temperature was 30℃and detection wavelength was set at 254 nm.The content of cAMP in Ziziphus jujube was determined by UPLC.Waters BEH C18(100 mm×2.1 mm,1.7μm)column was used with 0.05 mol/L KH2PO4 and methanol as mobile phase(8∶92)at the flow rate of 0.4 mL/min.The column temperature was 30℃and detection wavelength was set at 259 nm.Results A total of 14 common peaks were characterized,and the characteristic peaks were well-separated.The Guanosine,cAMP,5-hydroxymethylfurfural and Rutin were determined by reference substances.The determination of cyclic adenosine in 15 batches of Ziziphus jujube was 101~441μg/g.There was little difference between different habitats.It was higher in Shanxi,Henan and Gansu,and it was lower in Shandong and Hebei.Conclusion The present methodology meets the technical requirements,which can be a basis for the intrinsic quality control standard for Ziziphus jujube.
作者
曾杉
甘伟发
史紫娟
ZENG Shan;GAN Weifa;SHI Zijuan(Guangdong Medi-world Pharmaceutical Company Limited, Foshan 528303,China)
出处
《广东药科大学学报》
CAS
2020年第4期458-462,共5页
Journal of Guangdong Pharmaceutical University
