A novel quality by design approach for developing an HPLC method to analyze herbal extracts: A case study of sugar content analysis

Shao, Jingyuan; Cao, Wen; Qu, Haibin; Pan, Jianyang; Gong, Xingchu

doi:10.1371/journal.pone.0198515

Cited by 33 publications

(25 citation statements)

References 27 publications

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“…A Monte Carlo method was performed using a self-coded MATLAB program (R2016a, Version 9.0, The Math Works Inc., USA) to calculate the design space based on the speci c goals of process CQAs. The calculation process was introduced in previous work [33]. The acceptable ranges of the CQAs and the probability requirements for compliance are shown in Table 7.…”

Section: Control Strategy Of Astragali Radix Concentratesmentioning

confidence: 99%

“…The signals of Astragaloside IV and Astragaloside were detected by the ELSD detector. A typical chromatogram of Astragali radix supernatant was shown inFigure S1.The HPLC method developed by Shao et al was used to determine the contents of D-fructose and sucrose[33]. The HPLC system (1260, Agilent Technologies, USA) was equipped with an Alltech 2000ES ELSD detector.…”

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confidence: 99%

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Optimization of membrane dispersion ethanol precipitation process with a set of temperature control improved equipment

Pan

Tai

et al. 2020

Preprint

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Background Ethanol precipitation is an important separation and purification process in the traditional Chinese medicine (TCM) industry. However, ethanol precipitation process suffers from loss of active ingredients, low batch-to-batch consistency of supernatant composition, and long standing time. These problems are mainly caused by low efficient equipment and imperfect control strategy. Methods In the present study, a membrane dispersion ethanol precipitation device which can achieve rapid cooling was developed for Astragali radix ethanol precipitation. Ethanol precipitation process was optimized according to Quality by design concept. To identify critical material attributes (CMAs), ten batches of Astragali radix was used to prepare concentrates. Definitive screening design was used to investigate the relationships among critical process parameters, CMAs, and process critical quality attributes (CQAs). Results Calycosin-7-O-β-D-glucoside content, the sucrose content, and the electrical conductivity were found to be CMAs after the correlation analysis and stepwise regression modelling. Quadratic models were developed and design space was calculated according to the probability of attaining process CQA standards. A material quality control strategy was proposed. High quality and low quality Astragali radix concentrates can be discriminated by the inequalities. Low quality Astragali radix concentrates should not be released for ethanol precipitation process directly. Verification experiment results indicated accurate models and reliable design space. Conclusions The temperature control method and control strategy in this study are effective and promising for ethanol precipitation process of other TCMs or foods.

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Section: Control Strategy Of Astragali Radix Concentratesmentioning

confidence: 99%

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confidence: 99%

Optimization of membrane dispersion ethanol precipitation process with a set of temperature control improved equipment

Pan

Tai

et al. 2020

Preprint

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“…To estimate which parameters were significant for response values, the standard partial regression coefficient method was used to evaluate the results of Plackett-Burman experimental design and select CMPs [29]. Firstly, the response values were standardized according to Eq (1).…”

Section: Data Processingmentioning

confidence: 99%

Development and optimization of HPLC-MS method for simultaneous determination of four terpene trilactones in Ginkgo biloba leaf extracts based on Quality by Design principles

Zhang

Wang

et al. 2020

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Background Ginkgo biloba leaf extract (EGBL) is one of the most commonly used and most studied herbal medicines around the world. Taking into account that previously reported HPLC-ELSD methods for terpene trilactones determination in EGBL are time-consuming with complicated sample preparation, it is reasonable and meaningful to developing a simple, sensitive and robust HPLC-MS method based on a novel analytical quality by design (AQbD) approach. Methods Firstly, analytical target profile (ATP) and systematic risk analysis were carried out to identify potential critical method attributes (CMAs) and critical method parameters (CMPs). Secondly, CMPs were identified using a standard partial regression coefficient method. Thirdly, Box-Behnken design (BBD) was employed to establish the quantitative relationship between CMAs and CMPs. Fourthly, the Monte Carlo simulation method was used to build hypercube design space. Then, the verification experiments were performed. Fifthly, the optimized method was validated and utilized. Finally, the paired t test was used to compare the developed method with HPLC-ELSD. Results After the screening experiments, flow rate of mobile phase, the proportion of formic acid in the mobile phase, gas flow rate and gas temperature were identified as CMPs. Models to quantitatively describe the relationship between CMAs and CMPs were built. The operational hypercube design spaces of the HPLC-MS method for terpene trilactones analysis in EGBL were successfully calculated and found to be robust, which led to the analytical control strategy. The verification experiments were successfully performed within the design space and model was found to be accurate. The method had been successfully used for quality analysis of development batches of EGBL and obtained almost identical results to data determinated using HPLC. Conclusions In this work, an analytical control strategy for HPLC-MS method for terpene trilactones analysis in EGBL was developed using AQbD concepts, which is promising for application to other Chinese medicines. The developed HPLC-MS method is an alternative method for quantification of terpene trilactones in commercial EGBL and will be applicable throughout the life cycle of the product.

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“…To facilitate robustness studies of the HPLC method, an analytical quality‐by‐design (AQbD) approach was applied, which provided a systematic, risk‐based, and organized way to assess robustness . There have been many reports on HPLC method development and validation based on AQbD.…”

Section: Introductionmentioning

confidence: 99%

Establishing the chromatographic fingerprint of traditional Chinese medicine standard decoction based on quality by design approach: A case study of Licorice

Zhang

Wang

Chen

et al. 2019

J of Separation Science

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A novel analytical quality by design approach for developing a chromatographic fingerprint was established for analyzing complex traditional Chinese medicine, using a licorice standard decoction as an example. Considering the characteristics of integrity and ambiguity, the resolution of eight common peaks, total peak number, capacity factor distributions, and peak purity were selected as potential critical method attributes for assessing the quality of the chromatographic fingerprint. A central composite design was used to evaluate the relationship between critical method attributes and critical method parameters, including column temperature, wavelength, flow rate, formic‐acid concentration, and gradient parameters. A standard probability method was employed to calculate the design space of the fingerprint analysis parameters and evaluate the robustness of the methodology. The optimized high‐performance liquid chromatography fingerprint conditions were acetonitrile and 0.1% formic acid water gradient elution (0‐5 min, 5–19% A; 5–10 min, 19% A; 10–50 min, 19–42% A; 50–54 min, 42–100% A; 54–60 min, 100% A), column temperature 25±5°C, detection wavelength 265 nm. The design space of fingerprint analytical method based on the analytical quality by design approach not only met the requirements of the fingerprint analysis, but also improved the robustness and applicability of the fingerprint method.

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A novel quality by design approach for developing an HPLC method to analyze herbal extracts: A case study of sugar content analysis

Cited by 33 publications

References 27 publications

Optimization of membrane dispersion ethanol precipitation process with a set of temperature control improved equipment

Optimization of membrane dispersion ethanol precipitation process with a set of temperature control improved equipment

Development and optimization of HPLC-MS method for simultaneous determination of four terpene trilactones in Ginkgo biloba leaf extracts based on Quality by Design principles

Establishing the chromatographic fingerprint of traditional Chinese medicine standard decoction based on quality by design approach: A case study of Licorice

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