中国中药杂志

2015, v.40(10) 1845-1849

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田蓟苷的分离制备与香青兰子药材质量标准研究
Separation and authentication of tilianin and quality standards of semen of Dracocephalum moldavia

程雪梅;马亭云;苏来曼·哈力克;穆丹丹;田芳;侴桂新;王峥涛;王长虹;
CHENG Xue-mei;MA Ting-yun;SU Ley-man·Ha-lik;MU Dan-dan;TIAN Fang;CHOU Gui-xin;WANG Zheng-tao;WANG Chang-hong;Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,The Ministry of Education Key Laboratory for Standardization of Chinese Medicines and State Administration of Traditional Chinese Medicine Key Laboratory for New Resources and Quality Evaluation of Chinese Medicine,Shanghai R&D Centre for Standardization of Chinese Medicine of Chinese Medicine;The Xinj

摘要(Abstract):

该文采用色谱和光谱技术从维药香青兰子中分离并鉴定田蓟苷,经HPLC面积归一法测定其纯度大于98%。采用硅胶SGF254薄层板上,以氯仿-甲醇(5∶1)为展开剂,采用三氯化铝为显色剂,可对香青兰子药材中的活性成分田蓟苷进行定性鉴别。以田蓟苷为指标,采用C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1%磷酸(25∶75)为流动相,330 nm为检测波长,对香青兰子药材进行定量分析。田蓟苷在0.617 2~123.44 mg·L-1线性关系良好,标准曲线方程为Y=33.773X-0.824 8(r=1),平均回收率为101.0%,RSD为3.7%,方法的日内和日间精密度均小于2%。11批香青兰子中的4批正品药材的质量分数在0.016~0.187 mg·g-1。所建立的定性和定量方法可用于维药香青兰子药材的质量控制。
Tilianin was separated and authenticated from the seeds of Dracocephalum moldavia,a Uygur medicine,by chromatographic technique and spectroscopic method. The purity of tilianin is more than 98% determined by HPLC area normalization method.Thin layer chromatography( TLC) method was used to separate tilianin from D. moldavia by mixture of chloroform-methanol( 5∶ 1) as a developing solvent on high performance silicagel precoated plate( SGF254) and using aluminium trichloride as a chromogenic agent for qualitative identification of D. moldavia. To establish a HPLC method for quantitative analysis of D. moldavia,tilianin was used as a quantitative marker and separated on a C18( 4. 6 mm × 250 mm,5 μm) column with acetonitrile-0. 1% formic acid( 25∶ 75) as the mobile phase and detected at 330 nm. The calibration curve of tilianin displayed ideal linearity over the range of 0. 617 2-123. 44 μg·m L-1with a regression equation of Y = 33. 773X-0. 824 8( r = 1). The average recovery of tilianin was 101. 0% with RSD of 3. 7%.The RSD values of intra-day and inter-day precision were less than 2%. The content of tilianin in 4 batches of the authenticated semen of D. Moldavia was between 0. 016 and 0. 187 mg·g-1. The qualitative and quantitative method established is suitable for the quality evaluation and assessment of semen of D. Moldavia.

关键词(KeyWords): 香青兰子;田蓟苷;薄层鉴别;高效液相色谱;质量标准
semen of Dracocephalum moldavia;Tilianin;TLC;HPLC;quality standard

Abstract:

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基金项目(Foundation): 上海市国内科技合作领域项目(14495800200);; 新疆维吾尔自治区科技支疆计划项目(2013911134,201130105-5);; 国家药品标准提高暨2015版药典科研任务(M39)资助

作者(Author): 程雪梅;马亭云;苏来曼·哈力克;穆丹丹;田芳;侴桂新;王峥涛;王长虹;
CHENG Xue-mei;MA Ting-yun;SU Ley-man·Ha-lik;MU Dan-dan;TIAN Fang;CHOU Gui-xin;WANG Zheng-tao;WANG Chang-hong;Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,The Ministry of Education Key Laboratory for Standardization of Chinese Medicines and State Administration of Traditional Chinese Medicine Key Laboratory for New Resources and Quality Evaluation of Chinese Medicine,Shanghai R&D Centre for Standardization of Chinese Medicine of Chinese Medicine;The Xinj

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