Yu Cui, Chen Xi Gu, Yuzhen Liu, Jing Fang, Yiwen Ding, Y Liu, Yunli Fu, Yuyang Li, Lei Wang, Weidong Chen, Liang Yao
ABSTRACT HuoXueJieGu decoction is a compound traditional Chinese medicine comprising over 10 distinct herbal ingredients. Clinically utilized for managing rheumatoid arthritis and other rheumatic conditions, its documented efficacy includes promoting blood circulation, resolving stasis, reducing swelling, alleviating pain, and facilitating bone healing. However, the ambiguous material basis of HuoXueJieGu decoction significantly impedes the advancement of its quality control protocols and in‐depth exploration of its underlying pharmacological mechanisms. To address this gap, a comprehensive analytical method was developed for the systematic characterization of the HuoXueJieGu decoction aqueous extract. This method utilized a gradient elution system with ACN and an aqueous solution of 0.1% formic acid as the mobile phase. A total of 143 compounds were identified in the HuoXueJieGu decoction aqueous extract in vitro, which were categorized as follows: 31 organic acids, 29 flavonoids, 15 amino acids, 14 phenylpropanoids, 14 phenols, 12 alkaloids, 11 sugars and glycosides, 8 terpenoids, and 9 others. Furthermore, 31 constituents were detected in the plasma, indicating their systemic absorption. Tissue distribution analysis revealed the presence of 24, 19, 23, 40, and 38 prototype compounds in the heart, liver, spleen, lung, and kidney, respectively. Furthermore, this study represents the first report on the systematic and rapid characterization of the chemical profile of HuoXueJieGu decoction. It is also the first to interpret the functional roles of its constituents within the framework of the traditional “monarch‐minister‐assistant‐guide” theory. These findings provide a crucial scientific basis for elucidating the material basis of its efficacy and for advancing its quality control standards.
{"title":"Simultaneous Determination of HuoXueJieGu Decoction Chemical Composition, Plasma Components, and Tissue Distribution by Ultra‐High‐Performance Liquid Chromatography‐Quadrupole‐Orbitrap Mass Spectrometry","authors":"Yu Cui, Chen Xi Gu, Yuzhen Liu, Jing Fang, Yiwen Ding, Y Liu, Yunli Fu, Yuyang Li, Lei Wang, Weidong Chen, Liang Yao","doi":"10.1002/sscp.70196","DOIUrl":"https://doi.org/10.1002/sscp.70196","url":null,"abstract":"ABSTRACT HuoXueJieGu decoction is a compound traditional Chinese medicine comprising over 10 distinct herbal ingredients. Clinically utilized for managing rheumatoid arthritis and other rheumatic conditions, its documented efficacy includes promoting blood circulation, resolving stasis, reducing swelling, alleviating pain, and facilitating bone healing. However, the ambiguous material basis of HuoXueJieGu decoction significantly impedes the advancement of its quality control protocols and in‐depth exploration of its underlying pharmacological mechanisms. To address this gap, a comprehensive analytical method was developed for the systematic characterization of the HuoXueJieGu decoction aqueous extract. This method utilized a gradient elution system with ACN and an aqueous solution of 0.1% formic acid as the mobile phase. A total of 143 compounds were identified in the HuoXueJieGu decoction aqueous extract in vitro, which were categorized as follows: 31 organic acids, 29 flavonoids, 15 amino acids, 14 phenylpropanoids, 14 phenols, 12 alkaloids, 11 sugars and glycosides, 8 terpenoids, and 9 others. Furthermore, 31 constituents were detected in the plasma, indicating their systemic absorption. Tissue distribution analysis revealed the presence of 24, 19, 23, 40, and 38 prototype compounds in the heart, liver, spleen, lung, and kidney, respectively. Furthermore, this study represents the first report on the systematic and rapid characterization of the chemical profile of HuoXueJieGu decoction. It is also the first to interpret the functional roles of its constituents within the framework of the traditional “monarch‐minister‐assistant‐guide” theory. These findings provide a crucial scientific basis for elucidating the material basis of its efficacy and for advancing its quality control standards.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"9 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/pdfdirect/10.1002/sscp.70196","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147381945","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
ABSTRACT Promethazine hydrochloride is a phenothiazine derivative and is used for the treatment of antihistamine, antipsychotic, antiemetic, analgesic, anticholinergic, and sedative. During the routine analysis of promethazine hydrochloride, an unknown broad peak appeared using the related substances method indicated in the US Pharmacopeia. The separation method was optimized, and an unknown peak at a level of 0.11% was detected. Further study showed that the impurity could be detected in both USP reference standard and tablet samples, with the levels of 0.01% and 0.11%, respectively. In order to identify and characterize the impurity, high performance liquid chromatography‐tandem mass spectrometry technology was conducted to propose the chemical structure. 1D and 2D NMR were used to confirm the chemical structure of the unknown impurity as 1‐(10 H ‐[3,10′‐biphenothiazin]‐10‐yl)‐ N , N ‐dimethylpropan‐2‐amine. The formation of the impurity during the synthesis route was illustrated. The current study provided an optimized method for the quality control of promethazine hydrochloride drug substance and dosage forms.
{"title":"Identification of a Novel Impurity in Promethazine Hydrochloride Drug Substance and Tablets Using LC‐MS and NMR","authors":"Feng Su, Yuxiu Lin, Wenkai Zhu, Guan Wang, Jianjun Li, Abdelghani Mahmoudi, Peixi Zhu","doi":"10.1002/sscp.70177","DOIUrl":"https://doi.org/10.1002/sscp.70177","url":null,"abstract":"ABSTRACT Promethazine hydrochloride is a phenothiazine derivative and is used for the treatment of antihistamine, antipsychotic, antiemetic, analgesic, anticholinergic, and sedative. During the routine analysis of promethazine hydrochloride, an unknown broad peak appeared using the related substances method indicated in the US Pharmacopeia. The separation method was optimized, and an unknown peak at a level of 0.11% was detected. Further study showed that the impurity could be detected in both USP reference standard and tablet samples, with the levels of 0.01% and 0.11%, respectively. In order to identify and characterize the impurity, high performance liquid chromatography‐tandem mass spectrometry technology was conducted to propose the chemical structure. 1D and 2D NMR were used to confirm the chemical structure of the unknown impurity as 1‐(10 H ‐[3,10′‐biphenothiazin]‐10‐yl)‐ N , N ‐dimethylpropan‐2‐amine. The formation of the impurity during the synthesis route was illustrated. The current study provided an optimized method for the quality control of promethazine hydrochloride drug substance and dosage forms.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 12","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147330489","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
ABSTRACT A cost‐effective and straightforward vortex‐assisted matrix solid phase dispersion (VA‐MSPD) method was developed for extracting phenolic compounds from Salvia miltiorrhiza . UIO‐66‐NH 2 and 7 mL of 79% methanol aqueous solution containing 478 mM ionic liquid ([BMIM][BF4]) were selected as the dispersing sorbent and eluent, respectively. The optimal conditions were determined as follows: sample‐to‐dispersant mass ratio of 3.5:1, grinding time of 4 min, a vortex time of 2 min. Based on these results, response surface methodology (RSM) was further employed to investigate the effects of three key factors (sample‐to‐dispersant mass ratio, ionic liquid concentration, and methanol volume fraction) and their interactions on phenolic acids extraction efficiency. In addition, the combination of matrix solid‐phase dispersion and high‐performance liquid chromatography (HPLC) permitted the determination of four major natural polyphenolic compounds, including danshensu, rosmarinic acid, salvianolic acid B, and salvianolic acid A. The method demonstrated good linearity, showing limit of detection (LOD) of 0.13–0.28 µg·mL −1 and limit of quantitation (LOQ) of 0.42–0.92 µg·mL −1 . The developed vortex‐assisted matrix solid phase dispersion (VA‐MSPD) method showed higher extraction efficiency, greater convenience, and reduced time, making it an excellent choice for analyzing active components in traditional Chinese medicinal herbs.
{"title":"Determination of Phenolic Acids in <i>Salvia miltiorrhiza</i> by Vortex‐Assisted Matrix Solid‐Phase Dispersion Coupled With High‐Performance Liquid Chromatography","authors":"Yu Zhao, Yuxin Wang, Qiao Gao","doi":"10.1002/sscp.70161","DOIUrl":"https://doi.org/10.1002/sscp.70161","url":null,"abstract":"ABSTRACT A cost‐effective and straightforward vortex‐assisted matrix solid phase dispersion (VA‐MSPD) method was developed for extracting phenolic compounds from Salvia miltiorrhiza . UIO‐66‐NH 2 and 7 mL of 79% methanol aqueous solution containing 478 mM ionic liquid ([BMIM][BF4]) were selected as the dispersing sorbent and eluent, respectively. The optimal conditions were determined as follows: sample‐to‐dispersant mass ratio of 3.5:1, grinding time of 4 min, a vortex time of 2 min. Based on these results, response surface methodology (RSM) was further employed to investigate the effects of three key factors (sample‐to‐dispersant mass ratio, ionic liquid concentration, and methanol volume fraction) and their interactions on phenolic acids extraction efficiency. In addition, the combination of matrix solid‐phase dispersion and high‐performance liquid chromatography (HPLC) permitted the determination of four major natural polyphenolic compounds, including danshensu, rosmarinic acid, salvianolic acid B, and salvianolic acid A. The method demonstrated good linearity, showing limit of detection (LOD) of 0.13–0.28 µg·mL −1 and limit of quantitation (LOQ) of 0.42–0.92 µg·mL −1 . The developed vortex‐assisted matrix solid phase dispersion (VA‐MSPD) method showed higher extraction efficiency, greater convenience, and reduced time, making it an excellent choice for analyzing active components in traditional Chinese medicinal herbs.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 11","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147332782","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
ABSTRACT The fatty oil in Sanzi Yangqin Decoction is a crucial medicinal ingredient found in this renowned traditional Chinese medicine formula for the treatment of chronic obstructive pulmonary disease (COPD). However, a disadvantage of the extraction process using the conventional decoction approach is the poor extraction rate. In this study, we employed network pharmacology to screen for active components for the treatment of COPD, and we optimized the extraction procedure of the fatty oil of Sanzi Yangqin Decoction with the Box–Behnken response surface test. Based on the single‐factor experiment and the Box–Behnken response surface test, the liquid chromatography‐triple quadrupole mass spectrometry method (LC‐MS/MS) to measure these four components has been constructed with the extraction time, extraction temperature, and liquid‐to‐feed ratio as examining factors and the composite scores of the extracted amounts of the four components as examining indexes. According to the results of the study, luteolin, arachidonic acid, sinoacutine, and sinapine thiocyanate have been selected as the analytes for determining the fat oil content of Sanzi Yangqin Decoction. The most effective extraction conditions were 4.1 h, 92°C, and a liquid‐to‐feed ratio of 10:1 mL/g, which achieved a composite score of 85.1. The methodological analysis of the LC‐MS/MS methodology demonstrated that the precision, repeatability, and sample recovery all proved effective, and the linear relationship was good within the range of the four constituents. The optimized Sanzi Yangqin Decoction fatty oil extraction process is reasonable and feasible. And the LC‐MS/MS content determination method is simple, rapid, sensitive, and specific. This work introduces an innovative approach to examining the fatty oils in Sanzi Yangqin Decoction.
{"title":"Optimization of the Fatty Oil Extraction Process of Sanzi Yangqin Decoction Based on Network Pharmacology and Quantitative LC‐MS/MS Methods","authors":"Wenya Xu, Hailing Wang, Yan Sun, Hao Li, Jue Song","doi":"10.1002/sscp.70105","DOIUrl":"https://doi.org/10.1002/sscp.70105","url":null,"abstract":"ABSTRACT The fatty oil in Sanzi Yangqin Decoction is a crucial medicinal ingredient found in this renowned traditional Chinese medicine formula for the treatment of chronic obstructive pulmonary disease (COPD). However, a disadvantage of the extraction process using the conventional decoction approach is the poor extraction rate. In this study, we employed network pharmacology to screen for active components for the treatment of COPD, and we optimized the extraction procedure of the fatty oil of Sanzi Yangqin Decoction with the Box–Behnken response surface test. Based on the single‐factor experiment and the Box–Behnken response surface test, the liquid chromatography‐triple quadrupole mass spectrometry method (LC‐MS/MS) to measure these four components has been constructed with the extraction time, extraction temperature, and liquid‐to‐feed ratio as examining factors and the composite scores of the extracted amounts of the four components as examining indexes. According to the results of the study, luteolin, arachidonic acid, sinoacutine, and sinapine thiocyanate have been selected as the analytes for determining the fat oil content of Sanzi Yangqin Decoction. The most effective extraction conditions were 4.1 h, 92°C, and a liquid‐to‐feed ratio of 10:1 mL/g, which achieved a composite score of 85.1. The methodological analysis of the LC‐MS/MS methodology demonstrated that the precision, repeatability, and sample recovery all proved effective, and the linear relationship was good within the range of the four constituents. The optimized Sanzi Yangqin Decoction fatty oil extraction process is reasonable and feasible. And the LC‐MS/MS content determination method is simple, rapid, sensitive, and specific. This work introduces an innovative approach to examining the fatty oils in Sanzi Yangqin Decoction.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 8","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/pdfdirect/10.1002/sscp.70105","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147332540","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
ABSTRACT Zingiberis rhizoma , acknowledged as a pivotal “Rhizome of Medicine and Food,” differentiating chemical markers among various parts of Z. rhizoma will be significant due to the diversity of pharmacological activity and the similarity of chemical profiles. Here, a novel ultrasonic‐synergistic reverse egg phosphatidylcholine vesicles extraction (URPVE) combined with ultrahigh‐performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS)‐based metabolomics method was developed for comparing chemical profile among Z. rhizoma , Zingiber officinale peel, and peeled ginger (PG). The extraction conditions of URPVE were optimized by single‐factor experiments and response surface method using Box–Behnken design. Through multivariate statistical analysis, the results suggested that a total of 52 metabolites were identified, of which curcumin and zingerone contributed to a significant decreasing trend after peeling, and gingerol and gingerdiol were the most in Z. rhizome , and diacetoxy‐8‐gingerdiol and acetoxy‐8‐gingerol were the characteristic components in PG. This study enriches the understanding of Z. rhizoma by offering insights into comprehensive utilization of its diverse parts and provides a high‐efficiency extraction for the low‐polarity compounds from plant source.
{"title":"Comprehensive Studies on the Development of Ultrasonic‐Synergistic Reverse Egg Phosphatidylcholine Vesicles Extraction and LC–MS/MS‐Based Metabolomics Methods for Differentiating Diverse Parts of <i>Zingiberis rhizoma</i>","authors":"Jiahao Li, Pengfei Yan, Yong Xin, Siming Han, Xiaotong Yang, Jie Du, Jiaxi Li, Chengye Yan, Zeyu Hou, Wei Wei, Huijun Xu","doi":"10.1002/sscp.70094","DOIUrl":"https://doi.org/10.1002/sscp.70094","url":null,"abstract":"ABSTRACT Zingiberis rhizoma , acknowledged as a pivotal “Rhizome of Medicine and Food,” differentiating chemical markers among various parts of Z. rhizoma will be significant due to the diversity of pharmacological activity and the similarity of chemical profiles. Here, a novel ultrasonic‐synergistic reverse egg phosphatidylcholine vesicles extraction (URPVE) combined with ultrahigh‐performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS)‐based metabolomics method was developed for comparing chemical profile among Z. rhizoma , Zingiber officinale peel, and peeled ginger (PG). The extraction conditions of URPVE were optimized by single‐factor experiments and response surface method using Box–Behnken design. Through multivariate statistical analysis, the results suggested that a total of 52 metabolites were identified, of which curcumin and zingerone contributed to a significant decreasing trend after peeling, and gingerol and gingerdiol were the most in Z. rhizome , and diacetoxy‐8‐gingerdiol and acetoxy‐8‐gingerol were the characteristic components in PG. This study enriches the understanding of Z. rhizoma by offering insights into comprehensive utilization of its diverse parts and provides a high‐efficiency extraction for the low‐polarity compounds from plant source.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 7","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147333655","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jun Dai, Zimeng Gu, Sungwoo Hong, Yujuan Wang, Wanjiao Wang, Zenggen Liu
ABSTRACT With the growing interest in the comprehensive utilization of medicinal plants to maximize their therapeutic potential, this study focused on flavonoid components in the leaves of Polygonatum cyrtonema , an important traditional Chinese medicinal herb. Traditionally, the roots of P. cyrtonema are used medicinally, while the potential value of its above‐ground parts, such as the leaves, remains underexplored. Preliminary research revealed that the leaves of P. cyrtonema exhibit remarkable antioxidant activity, suggesting the presence of abundant flavonoid compounds. To efficiently isolate these active components, a systematic separation method based on medium‐pressure preparative chromatography (MPLC) combined with preparative high‐performance liquid chromatography (Prep‐HPLC) was developed. Initially, flavonoids were enriched using MPLC with an MCI GEL R CHP20P stationary phase and a water/ethanol linear gradient elution for selective enrichment of target compounds. Subsequently, the enriched compounds were further separated by Prep‐HPLC on a Megress C18 column, guided by ultraviolet (UV) spectroscopy. This integrated strategy successfully isolated nine flavonoid compounds from the leaves of P. cyrtonema , seven of which are novel and reported for the first time, with purities exceeding 96%. Compared to traditional separation methods, the developed approach exhibits superior advantages in terms of visualization, systematicity, reproducibility, and efficiency. It not only provides a targeted and efficient means for the isolation of flavonoid compounds from P. cyrtonema leaves but also serves as a valuable reference for the separation of bioactive compounds from other medicinal plants.
摘要随着人们对药用植物的综合利用以最大限度地发挥其治疗潜力的兴趣日益浓厚，本研究重点研究了黄精叶中黄酮类化合物的成分。传统上，胞丝藤的根被用作药用，而其地上部分的潜在价值，如叶子，仍未得到充分开发。初步研究表明，胞浆叶具有显著的抗氧化活性，表明其含有丰富的类黄酮化合物。为了有效地分离这些活性成分，建立了一种基于中压制备色谱（MPLC）和制备高效液相色谱（Prep - HPLC）的系统分离方法。首先，采用MPLC富集，MCI GEL R CHP20P固定相和水/乙醇线性梯度洗脱选择性富集目标化合物。随后，在Megress C18柱上，紫外（UV）光谱引导下，用Prep‐HPLC进一步分离富集的化合物。该综合策略成功分离了9个黄酮类化合物，其中7个为首次报道的新化合物，纯度超过96%。与传统的分离方法相比，该方法在可视化、系统性、重现性和高效性等方面具有优势。该方法不仅为从胞丝藤叶中分离黄酮类化合物提供了一种有针对性的高效方法，而且为从其他药用植物中分离生物活性化合物提供了有价值的参考。
{"title":"Systematic and Efficient Isolation of Flavonoids by MPLC Combined With HPLC From <i>Polygonatum cyrtonema</i> Leaves","authors":"Jun Dai, Zimeng Gu, Sungwoo Hong, Yujuan Wang, Wanjiao Wang, Zenggen Liu","doi":"10.1002/sscp.70070","DOIUrl":"https://doi.org/10.1002/sscp.70070","url":null,"abstract":"ABSTRACT With the growing interest in the comprehensive utilization of medicinal plants to maximize their therapeutic potential, this study focused on flavonoid components in the leaves of Polygonatum cyrtonema , an important traditional Chinese medicinal herb. Traditionally, the roots of P. cyrtonema are used medicinally, while the potential value of its above‐ground parts, such as the leaves, remains underexplored. Preliminary research revealed that the leaves of P. cyrtonema exhibit remarkable antioxidant activity, suggesting the presence of abundant flavonoid compounds. To efficiently isolate these active components, a systematic separation method based on medium‐pressure preparative chromatography (MPLC) combined with preparative high‐performance liquid chromatography (Prep‐HPLC) was developed. Initially, flavonoids were enriched using MPLC with an MCI GEL R CHP20P stationary phase and a water/ethanol linear gradient elution for selective enrichment of target compounds. Subsequently, the enriched compounds were further separated by Prep‐HPLC on a Megress C18 column, guided by ultraviolet (UV) spectroscopy. This integrated strategy successfully isolated nine flavonoid compounds from the leaves of P. cyrtonema , seven of which are novel and reported for the first time, with purities exceeding 96%. Compared to traditional separation methods, the developed approach exhibits superior advantages in terms of visualization, systematicity, reproducibility, and efficiency. It not only provides a targeted and efficient means for the isolation of flavonoid compounds from P. cyrtonema leaves but also serves as a valuable reference for the separation of bioactive compounds from other medicinal plants.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 6","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147330982","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Xiwen He, Zhiwen Li, Zhang Li, Juan Zhao, F. Yu, Wenbin Gan
ABSTRACT Tea is one of the most popular beverages in the world. In tea plant ( Camellia sinensis ) cultivation, the application of pesticides and herbicides constitutes a common agricultural practice for integrated pest management and weed control. Researchers usually focus on the pesticide residues in tea itself and rarely study the pesticide residues in tea soup. This study presents a rapid quantitative analysis method for detecting 36 common pesticides in green tea soup. The method involves using effervescent‐assisted extraction combined with dispersive liquid–liquid microextraction. Pesticides in tea soup are extracted with nonanoic acid, and during the extraction process, sodium carbonate solution (Na 2 CO 3 solution) and sulfuric acid (H 2 SO 4 ) are added to produce carbon dioxide for auxiliary extraction. The solidified substances are then dissolved in methanol and analyzed using LC–MS/MS. This study revealed that the 36 target pesticides exhibited strong linear responses across a concentration range of 1–50 ng mL −1 , with correlation coefficients ( R 2 ) exceeding 0.99. The developed method demonstrated a limit of quantification (LOQ) of 0.1 µg L −1 , accompanied by recovery rates ranging from 76.3% to 101.4% and relative standard deviations (RSDs) below 6.7% across all validation parameters. This approach is cost‐effective, minimizes the use of organic reagents, and reduces environmental pollution. Overall, the combination of effervescent‐assisted extraction and dispersive liquid–liquid microextraction is efficient for detecting pesticides in tea soup, making it suitable for routine analysis of commonly used pesticides in green tea soup.
茶是世界上最受欢迎的饮料之一。在茶树（Camellia sinensis）种植中，农药和除草剂的应用是综合虫害管理和杂草控制的常见农业做法。研究人员通常关注茶叶本身的农药残留，而很少对茶汤中的农药残留进行研究。建立了一种快速定量检测绿茶中36种常见农药的方法。方法包括泡腾辅助萃取与分散液-液微萃取相结合。用壬酸提取茶汤中的农药，在提取过程中加入碳酸钠溶液（na2co3溶液）和硫酸（h2so4）产生二氧化碳辅助提取。然后将固化的物质溶解在甲醇中，使用LC-MS /MS进行分析。结果表明，在1 ~ 50 ng mL−1的浓度范围内，36种目标农药表现出较强的线性响应，相关系数（r2）均超过0.99。该方法的定量限（LOQ）为0.1µg L−1，回收率为76.3% ~ 101.4%，相对标准偏差（rsd）小于6.7%。这种方法具有成本效益，最大限度地减少了有机试剂的使用，并减少了环境污染。综上所述，泡腾辅助萃取和分散液液微萃取相结合的方法对茶汤中农药的检测是有效的，适用于绿茶中常用农药的常规分析。
{"title":"Rapid Determination of 36 Pesticide Residues in Tea Soup Using Dispersive Liquid–Liquid Microextraction Technology Based On Hydrophobic Fatty Acid Combined With Effervescent‐Assisted Extraction","authors":"Xiwen He, Zhiwen Li, Zhang Li, Juan Zhao, F. Yu, Wenbin Gan","doi":"10.1002/sscp.70037","DOIUrl":"https://doi.org/10.1002/sscp.70037","url":null,"abstract":"ABSTRACT Tea is one of the most popular beverages in the world. In tea plant ( Camellia sinensis ) cultivation, the application of pesticides and herbicides constitutes a common agricultural practice for integrated pest management and weed control. Researchers usually focus on the pesticide residues in tea itself and rarely study the pesticide residues in tea soup. This study presents a rapid quantitative analysis method for detecting 36 common pesticides in green tea soup. The method involves using effervescent‐assisted extraction combined with dispersive liquid–liquid microextraction. Pesticides in tea soup are extracted with nonanoic acid, and during the extraction process, sodium carbonate solution (Na 2 CO 3 solution) and sulfuric acid (H 2 SO 4 ) are added to produce carbon dioxide for auxiliary extraction. The solidified substances are then dissolved in methanol and analyzed using LC–MS/MS. This study revealed that the 36 target pesticides exhibited strong linear responses across a concentration range of 1–50 ng mL −1 , with correlation coefficients ( R 2 ) exceeding 0.99. The developed method demonstrated a limit of quantification (LOQ) of 0.1 µg L −1 , accompanied by recovery rates ranging from 76.3% to 101.4% and relative standard deviations (RSDs) below 6.7% across all validation parameters. This approach is cost‐effective, minimizes the use of organic reagents, and reduces environmental pollution. Overall, the combination of effervescent‐assisted extraction and dispersive liquid–liquid microextraction is efficient for detecting pesticides in tea soup, making it suitable for routine analysis of commonly used pesticides in green tea soup.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147333960","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Li Li, Zongyue Dong, Xiangyu Kong, Yan Ma, Kehao Yang, Na Xue, Hua Yuan, Xiaolin Qi, Chunhua Han, Kai Zhang
ABSTRACT Morinidazole belongs to the category of third‐generation nitroimidazole antibacterial drugs. In the course of morinidazole production, the mother liquor from the recrystallization process was subjected to analysis for the identification and detection of eight process‐related impurities through high‐performance liquid chromatography (HPLC). The eight impurities ( Imp‐A , Imp‐B , Imp‐C , Imp‐D , Imp‐E , Imp‐F , Imp‐G , and Imp‐H ) included three new impurities ( Imp‐A , Imp‐B , and Imp‐C ) that were previously unreported and one potential genotoxic impurity ( Imp‐H ). Purity separation from the recrystallization mother liquor was carried out using preparative HPLC. To characterize these eight process‐related impurities, high‐resolution mass spectrometry and nuclear magnetic resonance (NMR) spectroscopy were utilized, followed by direct synthesis. The retention times of the impurities were confirmed through co‐injection via HPLC. Additionally, Imp‐B , Imp‐C , and Imp‐G were detected in commercial morinidazole products. A detailed discussion was conducted on the possible pathways leading to the formation of these impurities. Furthermore, the toxicities of these compounds were predicted using ADMET/PK property prediction software based on artificial intelligence algorithm—ADMET Predictor. These results will provide technical support for the quality control of morinidazole.
{"title":"Isolation, Synthesis, and Identification of Process‐Related Impurities From Morinidazole","authors":"Li Li, Zongyue Dong, Xiangyu Kong, Yan Ma, Kehao Yang, Na Xue, Hua Yuan, Xiaolin Qi, Chunhua Han, Kai Zhang","doi":"10.1002/sscp.202400133","DOIUrl":"https://doi.org/10.1002/sscp.202400133","url":null,"abstract":"ABSTRACT Morinidazole belongs to the category of third‐generation nitroimidazole antibacterial drugs. In the course of morinidazole production, the mother liquor from the recrystallization process was subjected to analysis for the identification and detection of eight process‐related impurities through high‐performance liquid chromatography (HPLC). The eight impurities ( Imp‐A , Imp‐B , Imp‐C , Imp‐D , Imp‐E , Imp‐F , Imp‐G , and Imp‐H ) included three new impurities ( Imp‐A , Imp‐B , and Imp‐C ) that were previously unreported and one potential genotoxic impurity ( Imp‐H ). Purity separation from the recrystallization mother liquor was carried out using preparative HPLC. To characterize these eight process‐related impurities, high‐resolution mass spectrometry and nuclear magnetic resonance (NMR) spectroscopy were utilized, followed by direct synthesis. The retention times of the impurities were confirmed through co‐injection via HPLC. Additionally, Imp‐B , Imp‐C , and Imp‐G were detected in commercial morinidazole products. A detailed discussion was conducted on the possible pathways leading to the formation of these impurities. Furthermore, the toxicities of these compounds were predicted using ADMET/PK property prediction software based on artificial intelligence algorithm—ADMET Predictor. These results will provide technical support for the quality control of morinidazole.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"8 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-11-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/pdfdirect/10.1002/sscp.202400133","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147330519","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Shaileshkumar K. Koradia, Madhavi Patel, A. Sen, D. Sen, Prasanna Pradhan
The current study aims to develop and validate an analytical quality by design approach‐based high‐performance thin‐layer chromatographic (HPTLC) method for the analysis of Axitinib tablet samples. The chromatographic conditions in the TLC method were optimized using a three‐level full factorial design. The mobile phase composition and chamber saturation time served as the independent variables for optimization. The mobile phase used for TLC separation on pre‐coated aluminum plates with silica gel 60 F254 consisted of a mixture of ethyl acetate and isopropyl alcohol in a ratio of 9:1 (v/v). Axitinib was quantified at 330 nm using the densitometric method. Axitinib peak from tablet formulation was verified against the reference standard by comparing its single band at Rf 0.44 ± 0.02. Linearity was found to exist between 100 and 600 ng/band, with a correlation coefficient (r2) of 0.9978. The percentage recovery was obtained as 98.21%–99.05%. The system was validated by determining the parameters according to the guidelines of the International Council for Harmonization of Technical Conditions for Medical Products for Human Use. The proposed TLC method can be effectively applied to routine quality control of a pharmaceutical product.
{"title":"Analytical quality by design‐based thin‐layer chromatography method development and validation for assay and content uniformity testing of the anti‐neoplastic drug Axitinib in tablet formulation","authors":"Shaileshkumar K. Koradia, Madhavi Patel, A. Sen, D. Sen, Prasanna Pradhan","doi":"10.1002/sscp.202300176","DOIUrl":"https://doi.org/10.1002/sscp.202300176","url":null,"abstract":"The current study aims to develop and validate an analytical quality by design approach‐based high‐performance thin‐layer chromatographic (HPTLC) method for the analysis of Axitinib tablet samples. The chromatographic conditions in the TLC method were optimized using a three‐level full factorial design. The mobile phase composition and chamber saturation time served as the independent variables for optimization. The mobile phase used for TLC separation on pre‐coated aluminum plates with silica gel 60 F254 consisted of a mixture of ethyl acetate and isopropyl alcohol in a ratio of 9:1 (v/v). Axitinib was quantified at 330 nm using the densitometric method. Axitinib peak from tablet formulation was verified against the reference standard by comparing its single band at Rf 0.44 ± 0.02. Linearity was found to exist between 100 and 600 ng/band, with a correlation coefficient (r2) of 0.9978. The percentage recovery was obtained as 98.21%–99.05%. The system was validated by determining the parameters according to the guidelines of the International Council for Harmonization of Technical Conditions for Medical Products for Human Use. The proposed TLC method can be effectively applied to routine quality control of a pharmaceutical product.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"41 1","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139005643","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Bereket Tesfaye, A. Gure, Tsegaye Girma Asere, Toleshi Teshome, Yerosan Buzayo
An efficient analytical method has been developed based on dispersive solid‐phase extraction followed by gas chromatography‐mass spectrometry for the determinations of 13 organochlorine pesticides in fruit juice samples. In this method, dispersive solid phase extraction was used for the extraction of target analye using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent. Different experimental parameters affecting the extraction efficiencies the proposed method were carefully optimized. Under the optimum conditions, the calibration graphs were linear in the concentration range of 0.6–100 ng/mL with coefficients of determinations in the range of 0.9927–0.9991. The limits of detection and quantification determined as 3 and 10 times the signal‐to‐noise ratio were in the range of 0.01–0.03 and 0.6–1.0 ng/mL, respectively. Intra‐ and inter‐day precision studies of the proposed method, expressed as relative standard deviations, were in the range of 2.1%–9.2% and 2.2%–9.7%, respectively. The recoveries of the spiked fruit juices samples were in the range of 81.4%–105.1% with the corresponding relative standard deviations ranging from 1.0%–8.8%. In general, the proposed method demonstrated satisfactory analytical performance. Thus,it could be used as simple and attracive alternative method for the extraction of organochlorine pesticides from fruit juice sample and other related matrices.
{"title":"Dispersive solid‐phase extraction for the determination of organochlorine pesticides in fruit juice samples using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent","authors":"Bereket Tesfaye, A. Gure, Tsegaye Girma Asere, Toleshi Teshome, Yerosan Buzayo","doi":"10.1002/sscp.202300161","DOIUrl":"https://doi.org/10.1002/sscp.202300161","url":null,"abstract":"An efficient analytical method has been developed based on dispersive solid‐phase extraction followed by gas chromatography‐mass spectrometry for the determinations of 13 organochlorine pesticides in fruit juice samples. In this method, dispersive solid phase extraction was used for the extraction of target analye using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent. Different experimental parameters affecting the extraction efficiencies the proposed method were carefully optimized. Under the optimum conditions, the calibration graphs were linear in the concentration range of 0.6–100 ng/mL with coefficients of determinations in the range of 0.9927–0.9991. The limits of detection and quantification determined as 3 and 10 times the signal‐to‐noise ratio were in the range of 0.01–0.03 and 0.6–1.0 ng/mL, respectively. Intra‐ and inter‐day precision studies of the proposed method, expressed as relative standard deviations, were in the range of 2.1%–9.2% and 2.2%–9.7%, respectively. The recoveries of the spiked fruit juices samples were in the range of 81.4%–105.1% with the corresponding relative standard deviations ranging from 1.0%–8.8%. In general, the proposed method demonstrated satisfactory analytical performance. Thus,it could be used as simple and attracive alternative method for the extraction of organochlorine pesticides from fruit juice sample and other related matrices.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"7 1","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138982252","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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