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作 者:毕晓黎 刘梦云 陈伟韬 李养学 BI Xiaoli;LIU Mengyun;CHEN Weitao;LI Yangxue(Guangdong Province Engineering Technology Research Institute of Traditional Chinese Medicine, Guangdong Provincial Key Laboratory of Research and Development in Traditional Chinese Medicine, Guangzhou 510095, Guangdong, China;Guangdong Second Chinese Medicine Hospital Affiliated to Guangzhou University of Traditional Chinese Medicine, Guangzhou 510405, Guangdong, China)
机构地区:[1]广东省中医药工程技术研究院,广东省中医药研究开发重点实验室,广东广州510095 [2]广州中医药大学附属广东第二中医院,广东广州510405
出 处:《辽宁中医药大学学报》2018年第4期15-18,共4页Journal of Liaoning University of Traditional Chinese Medicine
基 金:广东省中医药局科研项目(20162008);创新中药研发平台建设项目(2017A070701017)
摘 要:目的:建立不同产地金边土鳖中3种核苷类成分定性鉴别与含量测定方法,为金边土鳖质量标准的制订提供实验参考。方法:采用薄层色谱法(TLC)对金边土鳖中尿嘧啶和次黄嘌呤进行定性鉴别;采用高效液相色谱法(HPLC)同时测定金边土鳖中尿嘧啶、尿囊素和次黄嘌呤3种核苷类成分,以Waters Spherisorb?STAR NH2(5μm,4.6 mm×250 mm)为色谱柱,以乙腈-水(95∶5)为流动相,等度洗脱,在柱温为30℃、波长为205 nm条件下,以0.8 m L·min-1的流速进行测定。结果:14批金边土鳖TLC色谱中尿嘧啶和次黄嘌呤斑点清晰、分离度好,可用于金边土鳖的定性鉴别;尿嘧啶、尿囊素和次黄嘌呤分别在0.1014-0.5410μg(r=0.9995)、0.0365-0.2920μg(r=0.9997)、0.0429-0.2385μg(r=0.9996)线性范围内线性关系良好;平均回收率分别为101.20%(RSD=1.60%)、101.47%(RSD=2.10%)、101.92%(RSD=3.40%)(n=9)。结论:所建立的3种核苷类成分定性定量分析方法操作简便、重复性好。Objective:To establish methods of qualitative identification and content determination of 3 nucleosides in Opisthoplatia orientalis Burm.,to provide reference for the quality standards of Opisthoplatia orientalis Burm. Methods:Uracil and hypoxanthine as the effective constituent of Opisthoplatia orientalisBurm. preparation was identified by TLC;And determined these three components by HPLC which was detected by a Waters Spherisorb?STAR NH2(5 μm,4.6 mm×250 mm),a mobile phase was acetonitrilewater solution(95∶5)in a isocratic elution manner,the temperature of column was 30℃,and detection wavelength was set at 205 nm,velocity of flow was 0.8 m L·min-1. Results:20 batches of Opisthoplatia orientalis Burm. TLC spots were clear and well separated,can be used for the qualitative identification of the Opisthoplatia orientalis Burm.;Uracil,allantoin and hypoxanthine displayed good linear relationships within the range of 0.1014-0.5410 μg(r=0.9995),0.0365-0.2920 μg(r=0.9997),0.0429-0.2385 μg(r=0.9996),and the average recoveries were 101.20%(RSD=1.60%),101.47%(RSD=2.10%),101.92%(RSD=3.40%)(n=9). Conclusion:The established methods for qualitative and quantitative analysis of 3 nucleosides are simple and reproducible.
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