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Optimized ultra-high-performance liquid chromatography tandem mass spectrometry method for detecting compositional changes in Eucommia ulmoides and Achyranthes bidentata paired decoctions in vitro and in vivo

Chen Chun, Lv Lei, Huang Yueying, Gao Mingzhu, Jiang Xue, Ge Xiaoying, Zheng Dan, Bao Leilei

Acta Chromatographica

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2024

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Vol. 36, no. 1

31--44

EN

Rationale: The bark of Eucommia ulmoides and the roots of Achyranthes bidentata are commonly used in traditional Chinese medicine, and their pairing appears in many traditional Chinese medicine formulas as a recognized compatible unit. However, the changes and interactions of the main components of these two formulas when paired remain unclear, and there is currently no standard or method for their quality control and assessment of pharmacological effects. Methods: An optimized ultra-high-performance liquid chromatography triple-quadrupole mass spectrometry (UHPLC-MS/MS) method was established for the simultaneous identification of 10 components in E. ulmoides and A. bidentata using in vitro and in vivo models. Tributyltin methacrylate was the internal standard solution, and the blood samples were treated by an organic solvent precipitation method. Gradient elution was conducted on a C₁₈ column at 25 °C with 0.1% formic acid water:acetonitrile as the mobile phase at a flow rate of 0.5 mL min⁻¹. Dynamic multiple response monitoring was performed in negative-ion mode using an Agilent Jet Stream electrospray ionization ion source. Results: In negative-ion detection mode, eucommiol exhibited a good response, and the isomers ginsenoside Ro and achyranthoside C could also be well separated. The developed method accurately detected the five components with a low blood content. Compared to controls, the levels of ginsenoside Ro, chikusetsusaponin Ⅳa, and achyranthoside C increased; the contents of geniposidic acid and pinoresinol diglucoside were unchanged; and the levels of eucommiol, geniposide, β-ecdysterone, genipin, and achyranthoside D decreased in vitro. In vivo, the contents of geniposidic acid, geniposide, pinoresinol diglucoside, and β-ecdysterone were reduced; the contents of eucommiol and ginsenoside Ro were unchanged; and those of achyranthoside D, chikusetsusaponin Ⅳa, and achyranthoside C increased compared to the corresponding levels in the internal control. Conclusions: A method for the quality control of the E. ulmoides-A. bidentata drug pair was established for the first time and the main components in 10 drug pairs could be determined simultaneously in vitro and in vivo. These findings show that the E. ulmoides and A. bidentata drug pair cause a compositional change, providing new ideas for the development of this combination to improve clinical efficacy.

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Simultaneous quantitation of 13 active components in SimiaoYong'an decoction using high-performance liquid chromatography with diode array detection

Zheng Liang, Wang Mengyue, Chen Zhong, Hou Jincai, Li Xiaobo

Acta Chromatographica

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2019

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Vol. 31, no. 3

216--221

EN

SimiaoYong'an decoction, a traditional Chinese medicine formula consisting of four herbs, has been widely used for the treatment of gangrene disease. However, its clinical application is restricted due to the lack of an effective quality control method that covers the main active compounds in the formula. In this study, a high-performance liquid chromatography with diode-array detection (HPLC–DAD) method was established for the simultaneous determination of 13 active compounds including harpagide, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, ferulic acid, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, angoroside C, harpagoside, cinnamic acid, glycyrrhizic acid, and ligustilide. Separation of these compounds was achieved using a Kromasil 100-5-C18 column with a gradient elution program consisting of acetonitrile and 0.4% phosphoric acid solution. The specificity, linearity, precision, repeatability, and accuracy tests were implemented to validate the method. The validated method was successfully applied for determination of 13 components from several finished batches of SimiaoYong'an decoction. The results demonstrated that the established method was accurate, reliable, and could be used as a suitable quality control method for the quantification of SimiaoYong'an decoction.

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Simultaneous determination of six alkaloids in Phellodendron amurense by high-performance liquid chromatography

Li C. D., Liu Y., Shi Y. P.

Acta Chromatographica

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2013

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Vol. 25, no. 2

275--285

EN

A high-performance liquid chromatography (HPLC) method has been developed for simultaneous determination of six alkaloids, i.e., (−)-(R)-platydesmin, noroxyhydrastinine, berberine, skimmianine, canthin-6-one, and pteleine in the herbal medicine of Phellodendron amurense Rupr. The optimal condition for extraction and separation was achieved with a linear mobile phase gradient prepared from 0.1% phosphoric acid and acetonitrile. The LODs and LOQs for the analytes ranged from 0.06 to 0.22 μg mL-1 and from 0.25 to 0.80 μg mL-1, respectively. The optimized method was applied to the determination of alkaloids in P. amurense Rupr. and was found to be efficient. This method can provide a scientific and technical platform to the manufacturers for setting up a quality control standard as well as to the public for quality and safety assurance of the proprietary traditional Chinese medicines.

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Neural network based identification of hysteresis in human meridian systems

Tan Y., Dong R., Chen H., He H.

International Journal of Applied Mathematics and Computer Science

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2012

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Vol. 22, no. 3

685-694

EN

Developing a model based digital human meridian system is one of the interesting ways of understanding and improving acupuncture treatment, safety analysis for acupuncture operation, doctor training, or treatment scheme evaluation. In accomplishing this task, how to construct a proper model to describe the behavior of human meridian systems is one of the very important issues. From experiments, it has been found that the hysteresis phenomenon occurs in the relations between stimulation input and the corresponding response of meridian systems. Therefore, the modeling of hysteresis in a human meridian system is an unavoidable task for the construction of model based digital human meridian systems. As hysteresis is a nonsmooth, nonlinear and dynamic system with a multi-valued mapping, the conventional identification method is difficult to be employed to model its behavior directly. In this paper, a neural network based identification method of hysteresis occurring in human meridian systems is presented. In this modeling scheme, an expanded input space is constructed to transform the multi-valued mapping of hysteresis into a one-to-one mapping. For this purpose, a modified hysteretic operator is proposed to handle the extremum-missing problem. Then, based on the constructed expanded input space with the modified hysteretic operator, the so-called Extreme Learning Machine (ELM) neural network is utilized to model hysteresis inherent in human meridian systems. As hysteresis in meridian system is a dynamic system, a dynamic ELM neural network is developed. In the proposed dynamic ELMneural network, the output state of each hidden neuron is fed back to its own input to describe the dynamic behavior of hysteresis. The training of the recurrent ELM neural network is based on the least-squares algorithm with QR decomposition.

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Simultaneous determination of ephedra alkaloids in traditional chinese medicines by high-performance liquid chromatography

Chen Y., Li X, Chen F., Zhu Q., Luo J.

Acta Chromatographica

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2012

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Vol. 24, no. 3

475--487

EN

A rapid, simple, and practical high-performance liquid chromatographic method (HPLC) was developed and validated for the simultaneous determination of norephedrine (NME), norpseudoephedrine (NMP), ephedrine (E), pseudoephedrine (PE), and methylephedrine (ME) in traditional Chinese medicines (TCM) which contained Ephedrae Herba (Ephedra). This analysis could be accomplished within 12.5 min with an Alltima Phenyl Column by isocratic elution using a mixture of KH2PO4 (20 mM)-acetonitrile (96:4, v/v) as the mobile phase at a flow-rate of 0.6 mL min−1 and a wavelength of 210 nm. This method was successfully applied to quantify ephedra alkaloids in both Ma-xing-gan-shi decoction and Ephedra decoction. The concentration of total ephedra alkaloids (4.62 mg mL−1) in Ma-xing-gan-shi decoction was much lower than that (7.10 mg mL−1) in Ephedra decoction. Furthermore, the concentration of NME, NMP, E, PE, and ME was significantly lower in Ma-xing-gan-shi decoction than that in Ephedra decoction, respectively. The method was easily acceptable and would be popular with most analytical laboratories.