{"title":"Stability Indicating RP-HPLC Method by QbD Approach and LC-MS Characterization of Degradation Products of Mifepristone.","authors":"Chandni Chandarana, Isha Juwarwala, Parixit Prajapati, Jaimin Kumar Patel","doi":"10.1093/chromsci/bmaf017","DOIUrl":"10.1093/chromsci/bmaf017","url":null,"abstract":"<p><p>A Stability indicating revered phase high performance liquid chromatography (RP-HPLC) method have been developed and validated for the estimation of Mifepristone. LC-MS Studies was carried out for identification of possible degradation products. A simple, rapid, accurate and precise stability indicating RP-HPLC method was developed for quantification of Mifepristone. The developed method used the mixture of methanol and water (88:12 v/v) as mobile phase at flow rate of 1 ml /min, which was optimized with the help of Quality by Design approach. Detection was carried out at 305 mm. The linearity of the proposed method was found in the concentration range of 5-25 μg/ml with regression coefficient (R2) of 0.996. LOD and LOQ were found to be 0.0324 and 0.0982 μg/ml, respectively. The recovery of the proposed method was found to be 98%-100%. The method was found to be precise and robust. The developed stability indicating RP-HPLC method was successfully applied for quantification of Mifepristone in pharmaceutical dosage form. The degradation products were characterized by LC-MS and the fragmentation pathways were proposed.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143753008","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Universal Quantitative Residual Solvent Analysis of Solids and Liquids Using a Full Evaporative Technique and Methanized Flame Ionization Detection.","authors":"Allison Ferranti, Taylor Hayward","doi":"10.1093/chromsci/bmaf014","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf014","url":null,"abstract":"<p><p>Residual solvent analysis is a common method used in the manufacturing of finished goods and pharmaceuticals to ensure the safety of the final product to the consumer. Typically, this involves a headspace sample introduction set up and then separation by gas chromatography (GC) with detection by a flame ionization detector (FID). This analysis can be very time consuming in sample preparation, calibration and analysis time. A full evaporative technique has been applied to both solid and liquid samples for the rapid vaporization of the solvent analytes, which is then introduced to a GC for separation. Additionally, a methanizer was used in line with the FID creating a uniform response for solvents of various heteroatoms and functionalities. This combination of full evaporative technique with a methanized-FID allows for the use of a single response factor for residual solvent analysis with demonstrated repeatability of ˂4%RSD. Spiked solid sample analysis shows recovery between 95% and 105% of solvents tested at ⁓2 μg of each analyte. Overall, the combination of full evaporative headspace sampling and methanized-FID can be applied to any sample matrix for any solvent used in manufacturing or production, making a universal method for residual solvent analysis.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143730251","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Vineeta V Khanvilkar, Shruti S Mandle, Prachi R Hande, Bhavin R Daka, Pratik P Jadhav
{"title":"RP-HPLC Method Development and Validation for Simultaneous Estimation of Berberine and Ursolic Acid in Formulation.","authors":"Vineeta V Khanvilkar, Shruti S Mandle, Prachi R Hande, Bhavin R Daka, Pratik P Jadhav","doi":"10.1093/chromsci/bmaf016","DOIUrl":"10.1093/chromsci/bmaf016","url":null,"abstract":"<p><p>Medicines used in ayurveda are typically made of many herbs or are polyherbals. Standardization of these medicines can be carried out by quantitative estimation of two or more of its markers simultaneously. Berberine and ursolic acid are two active markers which are present in an Ayurvedic formulation, Giloy Tulsi tablets. In the present research work, the Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for the simultaneous quantitative determination of berberine and ursolic acid from the formulation. With an RP Hemochrom C18 column, chromatographic separation was accomplished at 292 nm with eluent composed of methanol: acetonitrile (4:1, v/v) at a flow rate of 1.0 mL/min. The retention time of berberine and ursolic acid was obtained to be 1.5 ± 0.02 and 3.2 ± 0.02 min, respectively. A simple, rapid, accurate, specific, and robust analytical method was developed to estimate berberine and ursolic acid. This validated method can be used for routine quality control of ayurvedic formulations or herbal formulations having plants which contain berberine and ursolic acid.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143730255","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Preparation of Chiral Stationary Phase Based on 1,1'-bi-2-Naphthol for Chiral Enantiomer Separation.","authors":"Kun Fan, Rui Dong, Wenqing Hou, Canyu Yang, Kongchun Sun, LvJing Xu, Bingquan Chang, Desheng Wang, Congcong Zhang, Baochun Shen","doi":"10.1093/chromsci/bmae051","DOIUrl":"10.1093/chromsci/bmae051","url":null,"abstract":"<p><p>Two enantiomeric novel chiral stationary phases (CSPs) R-3-Amide-BINOL CSP (CSP-1) and S-3-Amide-BINOL CSP (CSP-2) were prepared using (R/S)-1,1'-bi-2-naphthol (BINOL) derivatives as chiral selectors. The structure of CSPs was characterized by nuclear magnetic resonance, scanning electron microscope and elemental analysis. Four chiral solutes were selected under normal phase HPLC conditions to evaluate the chiral separation ability of the two novel CSPs. The effects of mobile phase and acidic additives on enantiomeric separation were investigated. The combination of molecular docking simulation and experimental data has elucidated the crucial role of hydrogen bonds and π-π interactions formed between the analyte and CSP in chiral recognition, and different configurations of CSP can cause enantiomeric elution sequence reversal, indicating that the configuration of chiral selectors in CSP has a significant impact on chiral recognition ability.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142347578","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Gireesh M Ankad, Harsha Hegde, Iranna B Kotturshetti
{"title":"Ayurveda Detoxification Process Reduces Plumbagin from the Roots of Plumbago zeylanica L. - A RP-UFLC Analysis.","authors":"Gireesh M Ankad, Harsha Hegde, Iranna B Kotturshetti","doi":"10.1093/chromsci/bmae048","DOIUrl":"10.1093/chromsci/bmae048","url":null,"abstract":"<p><p>Ayurveda describes purification process of certain herbal drugs to reduce the toxicity and make them suitable for therapeutic purpose. The objective of the study was to evaluate the effect of detoxification process on plumbagin (PG) from the Plumbago zeylanica L. roots in marketed samples. It involved procurement of market samples from five states of India viz. Andhra Pradesh, Gujarat, Maharashtra, Madhya Pradesh and Punjab. The roots were purified in lime water (LW) as mentioned in Ayurveda. Reverse Phase Ultra-Flow Liquid Chromatography method was validated for identification of PG in unprocessed and processed roots and in the media (LW) used for purification after processing. The data was statistically analyzed by Analysis of Variance (ANOVA) and tested for significance by the Dunnett multiple comparison test. Results were expressed as mean ± SD mg/g dry weight of extract. The study indicated that the PG was reduced quantitatively after processing, while the amount of PG found in the LW was observed to be increased, indicating the leaching of PG during the purification process. In conclusion, the detoxification process eliminates PG from its roots and discloses the leaching effect in the media for the first time.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142140263","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Simple and Sensitive LC-MS/MS Method for Determination of Dapagliflozin and Its Major Metabolite in Human Plasma.","authors":"Zhijun Liu, Yanru Liu, Zhipeng Wang, Huiping Lu, Xiujing Zhu, Yuxi Bao, Bingyan Cai, Shouhong Gao, Xia Tao, Deduo Xu","doi":"10.1093/chromsci/bmaf019","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf019","url":null,"abstract":"<p><p>Dapagliflozin (DAPA), an inhibitor of sodium-dependent glucose cotransporter-2, has been created to treat individuals with type 2 diabetes mellitus. A method was developed and validated using high-performance liquid chromatography coupled to tandem mass spectrometry to aid in studying the connection between clinical effectiveness and concentration of DAPA and its primary metabolite dapagliflozin 3-O-glucuronide (D3OG) in human plasma. The two analytes were separated using the Waters XSELECT HSS T3 (2.1 × 100 mm, 3.5 μm; Waters Co., Milford, USA) chromatographic column, with a mobile phase flow rate of 0.3 mL/min. The elution program was performed after protein precipitation with methanol, which only required a 5-min duration. The extraction recovery was from 99.8 to 109% for DAPA and from 101 to 103% for D3OG. Validation of the method for detecting DAPA within the range of 5-50 ng/mL and D3OG within the range of 50-500 ng/mL demonstrated satisfactory inter- and intra-day precision and accuracy. The method was successfully developed and validated, and it was used to measure the levels of DAPA and D3OG in plasma samples from patients with type 2 diabetes mellitus.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144013080","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A New Method for the Quantification of Ethyl Sulfate and Isopropyl Sulfate Contents in Abacavir Sulfate by Ion Chromatography.","authors":"Venkata Ramana Reddy Junuthula, Surendra Babu Manabolu Surya, Naresh Kumar Katari, Chandrasekhar Reddy Kandati, Narendra Kumar Masani, Hemant Kumar Sharma","doi":"10.1093/chromsci/bmaf023","DOIUrl":"https://doi.org/10.1093/chromsci/bmaf023","url":null,"abstract":"<p><p>A predictable new method was developed and validated for the determination of ethyl sulfate (EtS) and isopropyl sulfate (IprS) contents in abacavir sulfate (ABS) drug substance by ion chromatography (IC). Ethyl alcohol, isopropyl alcohol and sulfuric acids were used in the manufacturing process of ABS. Therefore, there is a possibility to form respective sulfate impurities, i.e., EtSs and IprSs. Hence, a control strategy is required for EtS and IprS contents in ABS. Chromatographic separation of EtS and IprS contents in Abacavir sulfate was achieved on Metrosep A Supp 10 (250 mm × 4.0 mm) column and particles of 4.6 μm size. The mobile phase consists of buffer (3.2 mM Sodium carbonate and 1.0 mM of sodium bicarbonate) and acetonitrile in the ratio of 90:10 (v/v) with the flow rate of 0.6 mL min-1 by applying 30°C column oven temperature. The analytes were monitored by conductometric detector. The performance of the method was assessed by evaluating the specificity, linearity, sensitivity, precision, robustness and accuracy experiments. The limit of detection and limit of quantification values for EtS were 0.3 and 0.8 μg mL-1 and for IprS were 0.3 and 0.8 μg mL-1, respectively. The correlation co-efficient value of linearity experiment was 0.9999 for EtS, 0.9998 for IprS. The average recovery for EtS was 98.7% and for IprS was 100.9%. The method is robust for EtS and IprS contents and also specific from other common anions, i.e., chloride, bromide, nitrate, sulfate, methyl sulfate and methanesulfonic acids. The results proved that the validated method was simple and cost-effective for controlling EtS and IprS contents in ABS drug substance, and the method can be successfully applied in the quality control analysis.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144026661","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Xiaowei Shao, Nan Zhao, Yuping Li, Hongming Wang, Xueli Xu, Shuyue Wang
{"title":"Quality Evaluation of Qingwei Huanglian Pills Based on Fingerprint and Quantitative Analysis of Multi-Index Components Combined with Chemical Pattern Recognition Analysis.","authors":"Xiaowei Shao, Nan Zhao, Yuping Li, Hongming Wang, Xueli Xu, Shuyue Wang","doi":"10.1093/chromsci/bmaf018","DOIUrl":"10.1093/chromsci/bmaf018","url":null,"abstract":"<p><p>Qingwei Huanglian Pills (QHPs) is one of the most commonly used traditional Chinese medicine preparations for the treatment of mouth and tongue sores, but the existing quality evaluation standards have certain shortcomings and deficiencies. An effective and scientific quality evaluation method plays a vital role in medication safety. In this study, fingerprint and quantitative analysis of multi-index components combined with chemical pattern recognition analysis was used to comprehensively evaluate the quality of QHPs. The fingerprints of 15 batches of QHPs were generated and evaluated for similarity, with 10 characteristic peaks identified. Clustering hierarchical cluster analysis (HCA), principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) were employed to cluster and rank the 15 batches, while simultaneously identifying the components responsible for differences between batches. The HPLC fingerprints of QHPs, along with the content determination of 10 components, were established. Twenty-eight common peaks were identified, and 10 components were specified. The similarity between the 15 batches of samples ranged from 0.983 to 0.999. Cluster analysis and comprehensive score ranking of 15 batches of samples were performed by HCA and PCA, respectively, and 13 chemical markers affecting batch differences were screened by OPLS-DA. The method established here can serve as a reference for the quality evaluation and product quality control of QHPs.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":"63 4","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143752994","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A General Strategy to Rapid and Sensitive Determination of Five High Boiling Point Solvents in Pharmaceuticals by RP-HPLC Combined with Precipitation Method.","authors":"Chenxia Zhang, Zeyi Wu, Meiyan Qiu, Yanhua Li, Zhongqing Wang, Xiaomei Fan, Shaoyu Cai, Wanbing Rao","doi":"10.1093/chromsci/bmae057","DOIUrl":"10.1093/chromsci/bmae057","url":null,"abstract":"<p><p>The difficulty on determination of high boiling point solvents, always exist due to their low vapor pressure in headspace (HS) vial. What's worse, the commonly used GC diluents, such as N, N-dimethylacetamide, 1,3-dimethyl-2-imidazolidinone, dimethyl sulfoxide, N, N-dimethylformamide and N-methylpyrrolidone are often remained in HS instrument after frequent injection into HS, thus would result in terrible positive interference problem. In this work, a fast and sensitive HPLC method in combination with a sample precipitation method, was proposed for the determination of above five high boiling point solvents in drug substances within 14.5 min. The final method was validated with regard to limit of detection and limit of quantitation, precision, linearity and accuracy in accordance with ICH Q2 (R1). Finally, the proposed strategy was successfully applied for the analysis of high boiling point solvents used in three active pharmaceutical ingredients. The established generic strategy would provide another choice for the determination of high boiling point solvents in pharmaceuticals.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142621360","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ling-Di Wang, Jing-Yun Gao, Li-Ying Duan, Hai-Feng Pan
{"title":"Verifying the Equivalence of Hawthorn Leaves Standard Decoction and Formula Granules by LC-MS and Oxidative Stress Test.","authors":"Ling-Di Wang, Jing-Yun Gao, Li-Ying Duan, Hai-Feng Pan","doi":"10.1093/chromsci/bmad089","DOIUrl":"10.1093/chromsci/bmad089","url":null,"abstract":"<p><strong>Objective: </strong>To verify the equivalence of hawthorn leaves standard decoction and formula granules.</p><p><strong>Methods: </strong>In this experiment, liquid chromatograph mass spectrometer (LC-MS) was used to examine the chemical composition of hawthorn leaves standard decoction and formula granules, separately. In addition, oxidative stress test was used to explore the antioxidant capacity of them.</p><p><strong>Results: </strong>71 chemical components were identified by LC-MS. Among them, 64 and 56 compounds were identified in the standard decoction and formula granules, respectively. There were a total of 49 common components, with no significant difference in content. Oxidative stress test showed that hawthorn leaves standard decoction and formula granules had no obvious toxicity to human umbilical vein endothelial cells. Compared with the model group, the same dose of hawthorn leaves formula granule and standard decoction could inhibit the secretion of lactate dehydrogenase and malondialdehyde (P < 0.05), and increase the content of superoxide dismutase (P < 0.01), with no statistically significant difference.</p><p><strong>Conclusions: </strong>There is no significant difference in the main active ingredients between the standard decoction and the formula granules, and the antioxidant activity in vitro is equivalent, providing an important theoretical basis for the further development of hawthorn leaves formula granules.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2025-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138482424","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}