Online solid‐phase extraction with high‐performance liquid chromatography and mass spectrometry for the determination of five tannins in traditional Chinese medicine injections

Sun, Meng; Lin, Yuanyuan; Jie, Zhang; Wang, Sicen

doi:10.1002/jssc.201501037

J of Separation Science

2016

DOI: 10.1002/jssc.201501037

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Online solid‐phase extraction with high‐performance liquid chromatography and mass spectrometry for the determination of five tannins in traditional Chinese medicine injections

Meng Sun

Yuanyuan Lin

Zhang Jie

et al.

Abstract: A rapid analytical method based on online solid-phase extraction with high-performance liquid chromatography and mass spectrometry has been established and applied to the determination of tannin compounds that may cause adverse effects in traditional Chinese medicine injections. Different solid-phase extraction sorbents have been compared and the elution buffer was optimized. The performance of the method was verified by evaluation of recovery (≥40%), repeatability (RSD ≤ 6%), linearity (r(2) ≥ 0.993), and lim… Show more

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Cited by 7 publications

(1 citation statement)

References 26 publications

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“…The present study reveals that nutraceutical formulation with vitamins was chosen to develop analytical separation method using Soxhlet's extraction with acetone solvent followed by evaporation with a rotary evaporator and fluorescence detection [14][15][16][17] . The developed method is precise, linear, accurate, robust and stability indicating compared to other UV detection regular HPLC methods.…”

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confidence: 99%

Vitamin K2-4 and K2-7 Estimation in Nutraceutical Solid Dosage Forms by Post Column Derivatization with Fluorescence Detection

Karuppiah¹,

Basha²

2016

ijps

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A post column derivatization method for the estimation of fat soluble vitamins K 2 -4 and K 2 -7 was developed by reverse phase HPLC and validated as per ICH guidelines. The compounds were extracted by solvent extraction with acetone followed by evaporation in a rotary evaporator. The residue was dissolved in ethanol and injected in to a chromatograph consisting of C18 column (Waters symmetry, 150×4.6, 3.5 μ) and fluorescence detector. The derivatization reagent was prepared by dissolving 136 mg of zinc chloride, 40 mg of sodium acetate and 0.1 ml of glacial acetic acid in methanol. The mobile phase comprises of methanol:isopropyl alcohol:acetonitrile:zinc chloride buffer solution 850:90:50:10 with a flow rate of 1 ml/min. The overall percentage recoveries of five different levels were found to be 99.85 and 100.5%, respectively. The linearity of the analytical method was determined from 10% to 120% level and the linear regression coefficients were 0.9991 and 0.9995 which is well within the acceptance criteria of 0.999. The limits of detection and limits of quantification were determined based on signal to noise ratio. The established values were 0.050, 0.50 μg/ml and 0.005, 0.047 μg/ml which is much lesser than available literatue limits. The developed method can be more suitable for the estimation of K 2 -4 and K 2 -7 present in drug substances as well as drug product formulations.Key words: Post column derivatization, nutraceutical solid dosage forms, estimation of K 2 -4 and K 2 -7 by HPLC, zinc chloride buffer solution, analytical estimation Vitamin K 2 includes several subtypes; the two subtypes most studied are menaquinone-4 (menatetrenone, MK-4) and menaquinone-7 (MK-7). Vitamin K 2 -4 ( fig. 1a) is yellow coloured powder, molecular formula C 31 H 40 O 2, molecular weight 444.65 g/mol, soluble in acetone and ethyl alcohol [1] . Vitamin K 2 -7 ( fig. 1b) is light yellow microcrystalline powder, molecular formula C 46 H 64 O 2, molecular weight 648.99 g/mol, soluble in petroleum ether, acetone, ethyl alcohol and insoluble in water [1] . Vitamin K is used for the treatment of anticoagulantinduced prothrombin deficiency caused by warfarin [2][3][4] . The American Academy of Paediatrics recommends that vitamin K should be given to all new born babies as a single intramuscular dose to prevent vitamin K deficiency bleeding. In Japan, vitamin K 2 is used for the management of osteoporosis. The fermented soya product nattō is rich in menaquinone-7 [2][3][4] .Derivatization reaction with the reduction of zinc metal ions to isolate compounds of closely eluting peaks by chromatography is fast emerging tool for analytical separation. The dosage form formulated with two active ingredients such as K 2 -4 and K 2 -7 along with excipients is very challenging effort to separate from its moiety. In order to separate the K series vitamins with almost same structural properties, the post column derivatization technique with fluorescence detection was used. The reduction mechanism of components with zinc chloride derivatizatio...

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confidence: 99%

Vitamin K2-4 and K2-7 Estimation in Nutraceutical Solid Dosage Forms by Post Column Derivatization with Fluorescence Detection

Karuppiah¹,

Basha²

2016

ijps

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The human mast cell line‐1 cell membrane chromatography coupled with HPLC‐ESI‐MS/MS method for screening potentical anaphylactic components from chuanxinlian injection

Lin

Wang

Hou

et al. 2017

Biomedical Chromatography

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Chuanxinlian injection is a traditional Chinese medicine injection widely used in China to treat sore throat, cough and dysentery, although a high occurrence of severe adverse reactions has been reported in clinical practice in recent years. In the present study, a human mast cell line-1 cell membrane chromatography coupled with HPLC-ESI-MS/MS method was established to screen and identify potentical anaphylactic components in chuanxinlian injection, and the dehydroandrographolide was identified as a potential anaphylactic component. In vitro anaphylactic assay showed that intracellular Ca concentration clearly increased under dehydroandrographolide (100 μm) treatment. β-Hexosaminidase and histamine release in human mast cell line-1 cells were both markedly enhanced with increased concentrations of dehydroandrographolide, confirming the anaphylactic activity of dehydroandrographolide. The application for chuanxinlian injection in this study suggested that the developed human mast cell line-1 cell membrane chromatography coupled with HPLC-ESI-MS/MS system may be effective and rapid for screening the potentical anaphylactic components from complex samples.

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On-line enrichment and determination of aristolochic acid in medicinal plants using a MOF-based composite monolith as adsorbent

Zhang

Liu

Han

et al. 2020

Journal of Chromatography B

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Online solid‐phase extraction with high‐performance liquid chromatography and mass spectrometry for the determination of five tannins in traditional Chinese medicine injections

Cited by 7 publications

References 26 publications

Vitamin K2-4 and K2-7 Estimation in Nutraceutical Solid Dosage Forms by Post Column Derivatization with Fluorescence Detection

Vitamin K2-4 and K2-7 Estimation in Nutraceutical Solid Dosage Forms by Post Column Derivatization with Fluorescence Detection

The human mast cell line‐1 cell membrane chromatography coupled with HPLC‐ESI‐MS/MS method for screening potentical anaphylactic components from chuanxinlian injection

On-line enrichment and determination of aristolochic acid in medicinal plants using a MOF-based composite monolith as adsorbent

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