杜仲树皮、新鲜叶片和杜仲愈伤组织块有效成分的含量测定

对杜仲树皮（市售）、杜仲新鲜叶片、杜仲幼苗各种愈伤组织块（茎段、幼叶、子房、花药经ＭＳ培养基附加生长调节素培养诱导而得的愈伤组织）的有效成分进行研究，证明它们有一些相同成分。用２，６－二氯酚靛酚滴定法测定了它们维生素Ｃ的含量；用紫外分光光度法测定了它们的桃叶珊瑚甙的含量；用薄层层析－分光光度法测定了它们的氯原酸的含量。     

A validation protocol for the HPTLC standardization of herbal products: application to the determination of acteoside in leaves of Plantago palmata Hook. f.s

Formal validation, that is the study of the analytical performances of a method, is recognized as the best safeguard against the generation and publication of data with low reliability.Although the topic of HPTLC validations has been largely investigated, there is still a need for a general validation method applicable whenever a blank matrix cannot be reconstituted, notably herbs and their extracts.This work proposes two validation schemes aiming at generate linearity, accuracy and precision data in a minimal number of HPTLC plates, taking the standardization of Plantago palmata as an example with both UV and visible (post-chromatographic derivatization with a sulphuric acid-vanillin reagent) detections. A major problem associated with HPTLC determinations is underlined, namely the low range of linearity which makes spiking studies quite difficult as care must be taken to avoid overloading, whereas keeping the analyte detectable in blank extracts and avoiding spikes too close to endogenous levels. A second problem is the use of general post-chromatographic derivatization reagents that compromise the selectivity of the method by reacting with compounds that may not be resolved from the compound of interest. The use of such reagents is clearly not without danger, especially given the relatively low resolution of planar chromatography.In conclusion, the retained validation protocol effectively yields the main validation data whereas allowing to pinpoint major analytical drawbacks. It was not possible to simultaneously validate aucubin and acteoside assays as both analytes are present at too different levels/detectabilities.     

A rapid and sensitive determination of aucubin in rat plasma by liquid chromatography-tandem mass spectrometry and its pharmacokinetic application

A sensitive, accurate, rapid and robust LC‐MS‐MS method for the quantification of aucubin, a major bioactive constituent of Aucuba japonica, Eucommia ulmoides and Plantago asiatica, was established and validated in rat plasma. Plasma samples were simply precipitated by adding methanol and the supernatant was chromatographed by a Diamonsil® C₁₈(2) column with the mobile phase comprising a mixture of 10 mm ammonium acetate in methanol and that in water with the ratio of 50:50 (v/v). Quantification of aucubin was performed by mass spectrometry in the multiple‐reaction monitoring mode with positive atmospheric ionization at m/z 364 → 149 for aucubin, and m/z 380 → 165 for catalpol (IS), respectively. The retention time was 2.47 and 2.44 min for aucubin and the IS, respectively. The calibration curve (10.0–30,000 ng/mL) was linear (r² > 0.99) and the lower limit of quantification was 10.0 ng/mL in the rat plasma sample. The method showed satisfactory results such as sensitivity, specificity, precision, accuracy, recovery, freeze–thaw and long‐term stability. This simple LC‐MS method was successfully applied in a pharmacokinetic study carried out in Sprague–Dawley rats after oral administration of aucubin at a single dose of 50 mg/kg. Herein the pharmacokinetic study of aucubin is reported for the first time. Copyright © 2011 John Wiley & Sons, Ltd.     

Synthesis of Acetal Dioxa-Cage Compounds Via Intramolecular Acetalization

An approach to tricyclic acetal dioxa-cage structure ( 1 ) and ( 2 ) involving intramolecular acetalization as the key protocol is reported.     

薄层色谱分离和分光光度法测定桃叶珊瑚甙

提出在冰醋酸－９５％乙醇（１：２,Ｖ／Ｖ）溶液中,以Ｅｐｓｔａｈｌ试剂为显色剂测定桃叶珊瑚甙的分光光度法。最大吸收波长为６０１ｎｍ。对于杜仲叶提取物中的桃叶珊瑚甙,以甲醇－氯仿－石油醚－乙酸乙酯为展开剂,用薄层色谱法予以分离,用分光光度法进行测定。     

杜仲中活性成分分析条件的优化研究

采用均匀设计法对对二甲氨基苯甲醛显色法测定桃叶珊瑚甙的显色条件进行了优化。建立了测定桃叶珊瑚甙的高灵敏方法 (ε=4 3× 10 4L·mol-1·cm-1) ,线性范围为 4 5～ 4 5 μg·mL-1,其灵敏度较文献报道提高 2 5倍。研究了显色剂用量、显色时间、显色温度、酸用量等因素对桃叶珊瑚甙显色反应的影响。该法应用于杜仲提取物中桃叶珊瑚甙的测定 ,结果令人满意。     

Quantitative Determination of Aucubin in Seven Plantago Species Using HPLC,HPTLC, and LC-ESI-MS Methods

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of aucubin in Plantago lanceolata. The analyses were carried out on Zorbax SB-C₁₈ column with an aqueous phosphoric acid and acetonitrile gradient. The correlation coefficient of calibration curve showed good linearity (r > 0.9995), with average recoveries between 96.7 and 104.5%. The developed method was applied for quantification in P. atrata, P. bellardii, P. coronopus, P. holosteum, P. reniformis, and P. schwarzenbergiana. The aucubin content in plant extracts was compared by HPLC, HPTLC, and LC-ESI-MS techniques and no significant differences between the conducted methods were observed.