Separation, Extraction and Purification of Natural Products from Plants

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Analysis of Natural Products and Pharmaceuticals".

Deadline for manuscript submissions: closed (20 November 2022) | Viewed by 26984

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Guest Editor
1. Pharmaceutical Informatics Institute, College of Pharmaceutical Science, Zhejiang University, Hangzhou 310058, China
2. Jinhua Institute of Zhejiang University, Jinhua 321016, China
Interests: traditional Chinese medicine quality control; pharmaceutical engineering
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Natural products include a large and diverse group of substances from various natural sources such as plants, bacteria, fungi, insects, arachnids, marine organisms and higher-order animals. Natural products have a long history of use as drugs, drug precursors and/or complementary health adjuvants. Most Chinese medicines and other traditional medicines are natural products.

Natural products are usually prepared through a series of processes such as extraction, precipitation and adsorption. Traditional natural product extraction and isolation techniques are time-consuming and expensive. It is particularly important to develop and improve the separation and extraction technology of natural products.

This Special Issue "Separation, Extraction and Purification of Natural Products from Plants" provides an opportunity to publish high-quality multidisciplinary research and reviews related to various aspects of natural product preparation methods, isolation, extraction and purification.

Dr. Xingchu Gong
Guest Editor

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Keywords

  • Chinese medicines
  • quality control
  • process analytical technology
  • quality by design
  • separation and purification
  • precipitation
  • chromatography
  • steam distillation
  • percolation
  • drying

Published Papers (13 papers)

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Research

Jump to: Review

18 pages, 12246 KiB  
Article
Optimization of Steam Distillation Process for Volatile Oils from Forsythia suspensa and Lonicera japonica according to the Concept of Quality by Design
by Xinying Chen, Dongyun Guo, Xingchu Gong, Na Wan and Zhenfeng Wu
Separations 2023, 10(1), 25; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10010025 - 01 Jan 2023
Cited by 1 | Viewed by 2083
Abstract
In this study, the process of steam distillation to collect volatile oils from Forsythia suspensa (F. suspensa) and Lonicera japonica (L. japonica) was optimized according to the concept of quality by design. First, the liquid/material ratio, distillation time, and [...] Read more.
In this study, the process of steam distillation to collect volatile oils from Forsythia suspensa (F. suspensa) and Lonicera japonica (L. japonica) was optimized according to the concept of quality by design. First, the liquid/material ratio, distillation time, and collection temperature were identified as critical process parameters by a review of the literature and single-factor experiments. Then, a Box–Behnken design was used to study the quantitative relationship between the three process parameters, two raw material properties, and the yield of volatile oil. A mathematical model was established with an R2 value exceeding 0.90. Furthermore, the design space of the volatile oil yield was calculated by a probability-based method. The results of a verification experiment showed that the model was accurate and the design space was reliable. A total of 16 chemical constituents were identified in the volatile oil from mixtures of F. suspensa and L. japonica. The content of β-pinene was the highest (54.75%), and the composition was similar to that of the volatile oil of F. suspensa. The results showed that when F. suspensa and L. japonica were distilled together, the main contribution to the volatile oil was from F. suspensa. The volatile oil yield from the combination of F. suspensa and L. japonica was not higher than that from L. japonica. Full article
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14 pages, 1498 KiB  
Article
Development of a Quantitative Chromatographic Fingerprint Analysis Method for Sugar Components of Xiaochaihu Capsules Based on Quality by Design Concept
by Jing Lan, Gelin Wu, Linlin Wu, Haibin Qu, Ping Gong, Yongjian Xie, Peng Zhou and Xingchu Gong
Separations 2023, 10(1), 13; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10010013 - 26 Dec 2022
Cited by 2 | Viewed by 1387
Abstract
Background: Xiaochaihu capsule is composed of seven traditional Chinese medicines. The pharmacopoeia only focuses on the quantitative detection of baicalin, which cannot fully reflect the quality of the preparation. Some medium polar components were used to establish the fingerprint of Xiaochaihu capsule, but [...] Read more.
Background: Xiaochaihu capsule is composed of seven traditional Chinese medicines. The pharmacopoeia only focuses on the quantitative detection of baicalin, which cannot fully reflect the quality of the preparation. Some medium polar components were used to establish the fingerprint of Xiaochaihu capsule, but there was no report on the strong polar components. Methods: A high performance liquid chromatography-corona charged aerosol detection technology was used to establish a fingerprint analysis method for Xiaochaihu capsules following an analytical quality by design approach. Definitive screening designed experiments were used to optimize the method parameters. A stepwise regression method was used to build quantitative models. The method operable design region was calculated using the experimental error simulation method. Plackett–Burman designed experiments were carried out to test robustness. Results: The contents of four components were simultaneously determined. There were seven common peaks in the fingerprint. The common peak area accounted for 91.72%. Both fingerprint and quantitative analysis methods were validated as applicable in the methodology study. The quantitative fingerprint analysis method for sugar components can fill the gap in the detection of strong polar components in the existing methods. It provides a new technology for the comprehensive overall evaluation of Xiaochaihu capsule. Full article
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11 pages, 2565 KiB  
Article
In-Line Vis-NIR Spectral Analysis for the Column Chromatographic Processes of the Ginkgo biloba L. Leaves. Part II: Batch-to-Batch Consistency Evaluation of the Elution Process
by Wenlong Li, Xi Wang, Houliu Chen, Xu Yan and Haibin Qu
Separations 2022, 9(11), 378; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9110378 - 18 Nov 2022
Viewed by 1300
Abstract
An in-line monitoring method for the elution process of Ginkgo biloba L. leaves using visible and near-infrared spectroscopy in conjunction with multivariate statistical process control (MSPC) was established. Experiments, including normal operating batches and abnormal ones, were designed and carried out. The MSPC [...] Read more.
An in-line monitoring method for the elution process of Ginkgo biloba L. leaves using visible and near-infrared spectroscopy in conjunction with multivariate statistical process control (MSPC) was established. Experiments, including normal operating batches and abnormal ones, were designed and carried out. The MSPC model for the elution process was developed and validated. The abnormalities were detected successfully by the control charts of principal component scores, Hotelling T2, or DModX (distance to the model). The results suggested that the established method can be used for the in-line monitoring and batch-to-batch consistency evaluation of the elution process. Full article
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18 pages, 2097 KiB  
Article
Development and Validation of a Near-Infrared Spectroscopy Method for Multicomponent Quantification during the Second Alcohol Precipitation Process of Astragali radix
by Wenlong Li, Yu Luo, Xi Wang, Xingchu Gong, Wenhua Huang, Guoxiang Wang and Haibin Qu
Separations 2022, 9(10), 310; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9100310 - 14 Oct 2022
Cited by 2 | Viewed by 1289
Abstract
The objective of this study was to develop and validate a near-infrared (NIR) spectroscopy based method for in-line quantification during the second alcohol precipitation process of Astragali radix. In total, 22 calibration experiments were carefully arranged using a Box–Behnken design. Variations in [...] Read more.
The objective of this study was to develop and validate a near-infrared (NIR) spectroscopy based method for in-line quantification during the second alcohol precipitation process of Astragali radix. In total, 22 calibration experiments were carefully arranged using a Box–Behnken design. Variations in the raw materials, critical process parameters, and environmental temperature were all included in the experimental design. Two independent validation sets were built for method evaluation. Validation set 1 was used for optimization. Different spectral pretreatments were compared using a “trial-and-error” approach. To reduce the calculation times, the full-factorial design was applied to determine the potential optimal combinations. Then, the best parameters for the pretreatment algorithms were compared and selected. Partial least squares (PLS) regression models were obtained with low complexity and good predictive performance. Validation set 2 was used for a thorough validation of the NIR spectroscopy method. Based on the same validation set, traditional chemometric validation and validation using accuracy profiles were conducted and compared. Conventional chemometric parameters were used to obtain the overall predictive capability of the established models; however, these parameters were insufficient for pharmaceutical regulatory requirements. Then, the method was fully validated according to the ICH Q2(R1) guideline and using the accuracy profile approach, which enabled visual and reliable representation of the future performances of the analytical method. The developed method was able to determine content ranges of 8.44–39.8% at 0.541–2.26 mg/mL, 0.118–0.502 mg/mL, 0.220–0.940 mg/mL, 0.106–0.167 mg/mL, 0.484–0.879 mg/mL, and 0.137–0.320 mg/mL for total solid, calycosin glucoside, formononetin glucoside, 9, 10-dimethoxypterocarpan glucopyranoside, 2′-dihydroxy -3′, 4′-dimethoxyisoflavan glucopyranoside, astragloside II, and astragloside IV, respectively. These ranges were specific to the early and middle stages of the second alcohol precipitation process. The method was confirmed to be capable of achieving an in-line prediction with a very acceptable accuracy. The present study demonstrates that accuracy profiles offer a potential approach for the standardization of NIR spectroscopy method validation for traditional Chinese medicines (TCMs). Full article
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18 pages, 4669 KiB  
Article
Inhibitory Effect and Mechanism of Dill Seed Essential Oil on Neofusicoccum parvum in Chinese Chestnut
by Tian-Tian Liu, Lin-Jing Gou, Hong Zeng, Gao Zhou, Wan-Rong Dong, Yu Cui, Qiang Cai and Yu-Xin Chen
Separations 2022, 9(10), 296; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9100296 - 09 Oct 2022
Cited by 5 | Viewed by 1690
Abstract
The chestnut postharvest pathogen Neofusicoccum parvum (N. parvum) is an important postharvest pathogen that causes chestnut rot. Chestnut rot in postharvest reduces food quality and causes huge economic losses. This study aimed to evaluate the inhibitory effect of dill seed essential [...] Read more.
The chestnut postharvest pathogen Neofusicoccum parvum (N. parvum) is an important postharvest pathogen that causes chestnut rot. Chestnut rot in postharvest reduces food quality and causes huge economic losses. This study aimed to evaluate the inhibitory effect of dill seed essential oil (DSEO) on N. parvum and its mechanism of action. The chemical characterization of DSEO by gas chromatography/mass spectrometry (GC/MS) showed that the main components of DSEO were apiole, carvone, dihydrocarvone, and limonene. DSEO inhibited the growth of mycelium in a dose-dependent manner. The antifungal effects are associated with destroying the fungal cell wall (cytoskeleton) and cell membrane. In addition, DSEO can induce oxidative damage and intracellular redox imbalance to damage cell function. Transcriptomics analysis showed DSEO treatment induced differently expressed genes most related to replication, transcription, translation, and lipid, DNA metabolic process. Furthermore, in vivo experiments showed that DSEO and DSEO emulsion can inhibit the growth of fungi and prolong the storage period of chestnuts. These results suggest that DSEO can be used as a potential antifungal preservative in food storage. Full article
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15 pages, 3246 KiB  
Article
Optimization of Steam Distillation Process and Chemical Constituents of Volatile Oil from Angelicaesinensis Radix
by Na Wan, Jing Lan, Zhenfeng Wu, Xinying Chen, Qin Zheng and Xingchu Gong
Separations 2022, 9(6), 137; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9060137 - 30 May 2022
Cited by 4 | Viewed by 2511
Abstract
In this study, the steam distillation process of volatile oil from Angelicaesinensis Radix was optimized according to the concept of quality-by-design. A homemade glass volatile oil extractor was used to achieve better cooling of the volatile oil. First, the soaking time, distillation [...] Read more.
In this study, the steam distillation process of volatile oil from Angelicaesinensis Radix was optimized according to the concept of quality-by-design. A homemade glass volatile oil extractor was used to achieve better cooling of the volatile oil. First, the soaking time, distillation time, and liquid–material ratio were identified as potential critical process parameters by consulting the literature. Then, the three parameters were investigated by single factor experiments. The volatile oil yield increased with the extension in the distillation time, and first increased and then decreased with the increase in soaking time and liquid–material ratio. The results confirmed that soaking time, distillation time, and liquid–material ratio were all critical process parameters. The kinetics models of volatile oil distillation from Angelicaesinensis Radix were established. The diffusion model of spherical particle was found to be the best model and indicated that the major resistance of mass transfer was the diffusion of volatile oil from the inside to the surface of the medicinal herb. Furthermore, the Box–Behnken experimental design was used to study the relationship between the three parameters and volatile oil yield. A second-order polynomial model was established, with R2 exceeding 0.99. The design space of the volatile oil yield was calculated by a probability-based method. In the verification experiments, the average volatile oil yield reached 0.711%. The results showed that the model was accurate and the design space was reliable. In this study, 21 chemical constituents of volatile oil from Angelicaesinensis Radix were identified by gas chromatograph-mass spectrometer(GC-MS), accounting for 99.4% of the total volatile oil. It was found that the content of Z-ligustilide was the highest, accounting for 85.4%. Full article
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17 pages, 5042 KiB  
Article
Enantiomeric Separation and Molecular Modelling of Bioactive 4-Aryl-3,4-dihydropyrimidin-2(1H)-one Ester Derivatives on Teicoplanin-Based Chiral Stationary Phase
by Isabella Bolognino, Antonio Carrieri, Rosa Purgatorio, Marco Catto, Rocco Caliandro, Benedetta Carrozzini, Benny Danilo Belviso, Maria Majellaro, Eddy Sotelo, Saverio Cellamare and Cosimo Damiano Altomare
Separations 2022, 9(1), 7; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9010007 - 28 Dec 2021
Cited by 3 | Viewed by 1651
Abstract
The enantiomeric separation of 15 racemic 4-aryl-3,4-dihydropyrimidin-2(1H)-one (DHP) alkoxycarbonyl esters, some of which proved to be highly active as A2B adenosine receptor antagonists, was carried out by HPLC on ChirobioticTM TAG, a chiral stationary phase (CSP) bearing teicoplanin aglycone [...] Read more.
The enantiomeric separation of 15 racemic 4-aryl-3,4-dihydropyrimidin-2(1H)-one (DHP) alkoxycarbonyl esters, some of which proved to be highly active as A2B adenosine receptor antagonists, was carried out by HPLC on ChirobioticTM TAG, a chiral stationary phase (CSP) bearing teicoplanin aglycone (TAG) as the chiral selector. The racemic compounds were separated under polar organic (PO) conditions. Preliminarily, the same selectands were investigated on three different Pirkle-type CSPs in normal-phase (NP) conditions. A baseline separation was successfully obtained on TAG-based CSPs for the majority of compounds, some of which achieved high enantioselectivity ratios (α > 2) in contrast with the smaller α values (1–1.5) and the lack of baseline resolution observed with the Pirkle-type CSPs. In particular, the racemic tetrazole-fused DHP ester derivatives, namely compounds 8 and 9, were separated on TAG-based HPLC columns with noteworthy α values (8.8 and 6.0, respectively), demonstrating the potential of the method for preparative purposes. A competition experiment, carried out with a racemic analyte (6) by adding N-acetyl-d-alanine (NADA) to the mobile phase, suggested that H-bonding interactions involved in the recognition of the natural dipeptide ligand d-Ala-d-Ala into the TAG cleft should be critical for enantioselective recognition of 4-aryl DHPs by TAG. The X-ray crystal structure of TAG was elucidated at a 0.77 Å resolution, whereas the calculation of molecular descriptors of size, polar, and H-bond interactions, were complemented with molecular docking and molecular dynamics calculations, shedding light on repulsive (steric effects) and attractive (H-bond—polar and apolar) interactions between 4-aryl DHP selectands and TAG chiral selectors. Full article
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11 pages, 1200 KiB  
Article
Quality Distinguish of Red Ginseng from Different Origins by HPLC–ELSD/PDA Combined with HPSEC–MALLS–RID, Focus on the Sugar-Markers
by Qian Cheng, Shuhuan Peng, Fangyi Li, Pengdi Cui, Chunxia Zhao, Xiaohui Yan, Tongchuan Suo, Chunhua Wang, Yongzhi He and Zheng Li
Separations 2021, 8(11), 198; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8110198 - 27 Oct 2021
Cited by 4 | Viewed by 2252
Abstract
Red ginseng (RG) has been extensively utilized in Asian countries due to its pharmacological effects. For the quality evaluation of RG, small molecules, such as ginsenosides, have been widely considered as candidates of its quality markers (Q-markers), and various analytical techniques have been [...] Read more.
Red ginseng (RG) has been extensively utilized in Asian countries due to its pharmacological effects. For the quality evaluation of RG, small molecules, such as ginsenosides, have been widely considered as candidates of its quality markers (Q-markers), and various analytical techniques have been developed in order to identify these compounds. However, despite the efforts to analyze the hydrophobic constituents, it is worth pointing out that about 60% of the mass of RG is made of carbohydrates, including mono-, oligo- and polysaccharides. Consequently, the quality differentiation and identification of RG from the perspective of sugar-markers should be focused. High performance liquid chromatography and evaporative light scattering detector (HPLC–ELSD) method for the determination of disaccharides in RG was established. Furthermore, high performance size exclusion chromatography–multi-angle laser light scattering–refractive index detector (HPSEC–MALLS–RID) for the determination of molecular weight and high performance liquid chromatography photodiode array (HPLC–PDA) for the determination of compositional monosaccharides in RG polysaccharides were also established. HPLC–ELSD/PDA combined with HPSEC–MALLS–RID could be used to determine the contents of disaccharides, molecular weights, and compositional monosaccharides of RG polysaccharides, which could be used for quality control, and this is a new view on the sugar marker to quality differentiation of various origins of RG. Full article
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12 pages, 1342 KiB  
Article
The Separation and Purification of Ellagic Acid from Phyllanthus urinaria L. by a Combined Mechanochemical-Macroporous Resin Adsorption Method
by Zili Guo, Shuting Xiong, Yuanyuan Xie and Xianrui Liang
Separations 2021, 8(10), 186; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8100186 - 14 Oct 2021
Cited by 2 | Viewed by 2307
Abstract
Ellagic acid is a phenolic compound that exhibits both antimutagenic and anticarcinogenic activity in a wide range of assays in vitro and in vivo. It occurs naturally in some foods such as raspberries, strawberries, grapes, and black currants. In this study, a valid [...] Read more.
Ellagic acid is a phenolic compound that exhibits both antimutagenic and anticarcinogenic activity in a wide range of assays in vitro and in vivo. It occurs naturally in some foods such as raspberries, strawberries, grapes, and black currants. In this study, a valid and reliable method based on mechanochemical-assisted extraction (MCAE) and macroporous adsorption resin was developed to extract and prepare ellagic acid from Phyllanthus urinaria L. (PUL). The MCAE parameters, acidolysis, and macroporous adsorption resin conditions were investigated. The key MCAE parameters were optimized as follows: the milling time was 5 min, the ball mill speed was 100 rpm, and the ball mill filling rate was 20.9%. Sulfuric acid with a concentration of 0.552 mol/L was applied for the acidolysis with the optimized acidolysis time of 30 min and acidolysis temperature of 40 °C. Additionally, the XDA-8D macroporous resin was chosen for the purification work. Both the static and dynamic adsorption tests were carried out. Under the optimized conditions, the yield of ellagic acid was 10.2 mg/g, and the content was over 97%. This research provided a rapid and efficient method for the preparation of ellagic acid from the cheaply and easily obtained PUL. Meanwhile, it is relatively low-cost work that can provide a technical basis for the comprehensive utilization of PUL. Full article
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11 pages, 981 KiB  
Article
Studies on the Separation and Purification of the Caulis sinomenii Extract Solution Using Microfiltration and Ultrafiltration
by Xi Wang, Huimin Feng, Halimulati Muhetaer, Zuren Peng, Ping Qiu, Wenlong Li and Zheng Li
Separations 2021, 8(10), 185; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8100185 - 14 Oct 2021
Cited by 6 | Viewed by 2240
Abstract
The separation and purification process of alkaloids faces great challenges of pollution, high energy consumption and low continuity. In this study, the effects of ceramic microfiltration (MF) membrane (membrane pore size of 0.50 μm, 0.20 μm, 0.05 μm) and organic ultrafiltration (UF) membrane [...] Read more.
The separation and purification process of alkaloids faces great challenges of pollution, high energy consumption and low continuity. In this study, the effects of ceramic microfiltration (MF) membrane (membrane pore size of 0.50 μm, 0.20 μm, 0.05 μm) and organic ultrafiltration (UF) membrane (membrane molecular weight cut-off of 10 KDa and 1 KDa) on the separation and purification of Caulis sinomenii extract solution in pilot scale were studied. The cleaning effects of different cleaning methods (pure water, 1% HCl-NaOH, 1% sodium hypochlorite) were investigated. The experimental results indicated that 0.05 μm ceramic membrane and 1 kDa UF membrane have higher sinomenine hydrochloride (SH) permeabilities and total solids (TS) removal rates. The ceramic membrane was circulating cleaned by 1% sodium hypochlorite solution for 1 h; the membrane flux can be restored to more than 90% of the original, the membrane flux of 1 kDa UF membrane can be restored to 99.2% of the original by pure water washing. From the above study, the optimal technic parameters was determined in which 0.05 μm ceramic MF membrane and 1 kDa UF membrane were used to separate and purify the Caulis sinomenii extract solution to remove the invalid ingredients, and the two kinds of membranes were cleaned with 1% sodium hypochlorite solution and pure water, respectively, to keep satisfactory membrane fluxes. The study provided an environment-friendly alternative for the separation and purification of alkaloids in natural products, which has a good prospect for the industrial application. Full article
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16 pages, 2927 KiB  
Article
An Index for Quantitative Evaluation of the Mixing in Ethanol Precipitation of Traditional Chinese Medicine
by Yanni Tai, Jingjing Pan, Haibin Qu and Xingchu Gong
Separations 2021, 8(10), 181; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8100181 - 12 Oct 2021
Cited by 1 | Viewed by 1770
Abstract
(1) Background: Ethanol precipitation is widely used in the manufacturing traditional Chinese medicines (TCMs). Insufficient mixing of ethanol solution and concentrate usually results in the coating loss of active ingredients. However, there is no index for quantitative evaluation of the mixing in ethanol [...] Read more.
(1) Background: Ethanol precipitation is widely used in the manufacturing traditional Chinese medicines (TCMs). Insufficient mixing of ethanol solution and concentrate usually results in the coating loss of active ingredients. However, there is no index for quantitative evaluation of the mixing in ethanol precipitation. Therefore, this study aimed to define an index for quantitative evaluation of the mixing effect in ethanol precipitation of TCMs. (2) Methods: The concept and requirements of a mixing indicator were proposed. The mass percentage of concentrate fully mixed with ethanol solution (well-mixing ratio, WMR) was used as an index to evaluate the mixing effect. The formula for calculation of WMR was derived. The utility of the WMR was evaluated on stirring devices and a micromesh mixer. (3) Results: Increasing stirring speed, decreasing total solid content of the concentrate, and decreasing the diameter of the ethanol solution droplets all resulted in higher retention rates for lobetyolin and higher WMR. The WMR increased with the increasing flow rate of the concentrate and ethanol solution in the micromesh mixer. The mixing of ethanol solution and concentrate was better when using a micromesh mixer with a smaller internal mixing zone. The results revealed that WMR could be used to quantitatively characterize the mixing of concentrate and ethanol solution, although it has some limitations. (4) Conclusions: The proposed index WMR could guide quality control of the TCM ethanol precipitation process. This study represents a new contribution to improving ethanol precipitation equipment, optimizing process parameters, and enhanced properties of concentrate for TCM enterprises. Full article
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7 pages, 421 KiB  
Article
Determination of Genotoxic Azide Impurity in Cilostazol API by Ion Chromatography with Matrix Elimination
by Boglárka Páll, Zsuzsa Gyenge, Róbert Kormány and Krisztián Horváth
Separations 2021, 8(10), 162; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8100162 - 23 Sep 2021
Cited by 3 | Viewed by 2905
Abstract
Cilostazol is a commonly used active pharmaceutical ingredient (API) to treat and reduce the symptoms of intermittent claudication in peripheral vascular disease. Recently, it was found to be a potential medicine in the effective treatment of COVID-19. In addition to the positive effects [...] Read more.
Cilostazol is a commonly used active pharmaceutical ingredient (API) to treat and reduce the symptoms of intermittent claudication in peripheral vascular disease. Recently, it was found to be a potential medicine in the effective treatment of COVID-19. In addition to the positive effects of this API, genotoxic sodium azide is used in the synthesis of cilostazol that can appear in the API. In this work, a method was developed for the determination of sodium azide (as azide anion) in cilostazol API at 7.5 ppm limit level by using ion chromatography (IC) and liquid–liquid extraction (LLE) sample preparation. The liquid–liquid extraction allows the application of high sample concentrations. Because of the low limit concentration (7.5 ppm), 500 mg sample was dissolved in 5 mL solvent. By using LLE for sample preparation, the huge amount of cilostazol was omitted and column overload was avoided. The developed method was validated in accordance with the relevant guidelines. Specificity, accuracy, precision, limit of detection and limit of quantification parameters were evaluated. The calculated limit of detection was 0.52 ppm (S/N:3) and the limit of quantification was 1.73 ppm (S/N:10) for sodium azide. The recovery of the sodium azide was 102.4% and the prepared solutions were stable in the sample holder for 24 h. Full article
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Review

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15 pages, 1918 KiB  
Review
Research Progress on Quality Control Methods for Xiaochaihu Preparations
by Guangzheng Xu, Hui Wang, Yingqian Deng, Keyi Xie, Weibo Zhao and Xingchu Gong
Separations 2021, 8(11), 199; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8110199 - 01 Nov 2021
Cited by 3 | Viewed by 1631
Abstract
Xiaochaihu (XCH) is a classic Chinese medicine formula. XCH tablet, XCH granule, XCH capsule, and XCH effervescent tablet are included in the Chinese Pharmacopoeia. In this review, the formula and quality standards of XCH preparations at home and abroad were compared. The differences [...] Read more.
Xiaochaihu (XCH) is a classic Chinese medicine formula. XCH tablet, XCH granule, XCH capsule, and XCH effervescent tablet are included in the Chinese Pharmacopoeia. In this review, the formula and quality standards of XCH preparations at home and abroad were compared. The differences in manufacturing process of XCH preparations are discussed. The progress of research on the qualitative identification, quantitative detection and fingerprint chromatogram/specific chromatogram of XCH preparations was reviewed. The characteristic components of Pinelliae Rhizoma Praeparatum Cum Zingibere Et Alumine and Jujubae Fructus was rarely analyzed for XCH preparations. It is suggested that the specificity of drug quality detection methods should be improved. Considering drug safety and drug efficacy, it is suggested to set the upper and lower limits of the content of saikosaponins. The standards for heavy metals and other limited items for XCH preparations are also suggested to be set. Full article
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