{"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":"https://doi.org/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":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-09-27","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}
Rabab M Soliman, Yasmin Rostom, Yasmin M Fayez, Nadia M Mostafa, Hany H Monir
{"title":"Novel Green Chromatographic Approaches for Estimation of a Triple Common Cold Pharmaceutical Combination.","authors":"Rabab M Soliman, Yasmin Rostom, Yasmin M Fayez, Nadia M Mostafa, Hany H Monir","doi":"10.1093/chromsci/bmae050","DOIUrl":"https://doi.org/10.1093/chromsci/bmae050","url":null,"abstract":"<p><p>Nowadays, there is a strong interest in the scientific community in developing innovative methodologies within a green analytical chemistry framework. Herein, we introduce the first chromatographic approaches for the concurrent estimation of paracetamol (PAR), carbinoxamine (CRX), and pseudoephedrine (PSE) intended to relieve COVID-19 and common cold symptoms. The first method was thin layer chromatography (TLC) densitometry, which depends on the separation of the studied medications on TLC silica gel plates using ethyl acetate: methanol: ammonia (7.0: 3.0: 0.2, by volume) as the developing system, and were scanned at 208.0 nm. The data were linear in the ranges of 1-25 μg/band for PAR, 1-25 μg/band for PSE and 0.1-5 μg/band for CRX. The second method was reversed-phase high-performance liquid chromatography separation on a Kromasil C18 column using a mixture of 0.01 M phosphate buffer containing 0.1% triethylamine (pH 3.5) adjusted with orthophosphoric acid and ethanol at a flow rate of 1.0 mL/min in a gradient program. The separated peaks were detected at 215.0 nm over a concentration range of 10-250 μg/mL for PAR, 5-35 μg/mL for PSE, and 0.5-25 μg/mL for CRX. Both approaches were validated according to International Conference on Harmonization (ICH) guidelines. Finally, the impact of these methods on the environment was evaluated by many tools.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-09-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142347577","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 GC–MS Method for Determination of β-Propiolactone Residues in Inactivated Covid-19 Vaccines","authors":"Seyedeh Zohreh Mirjalili, Zahra Tamiji, Mehrnoosh Shirangi, Mohsen Amini","doi":"10.1093/chromsci/bmae049","DOIUrl":"https://doi.org/10.1093/chromsci/bmae049","url":null,"abstract":"β-propiolactone is a common inactivator agent used in vaccines. Due to β-propiolactone carcinogenicity, complete hydrolysis of it is necessary to prevent cytotoxicity in mammalian cells. As a result, more attention should be paid to it at the clinic, and it is important to measure its trace amounts. β-propiolactone analysis is challenging due to its instability. A simple and fast gas chromatography–mass spectrometry method was developed for quantitation of residual β-propiolactone in inactivated coronavirus disease 2019 (Covid-19) vaccines. Caprolactone was used as an internal standard in sample solutions; the analysis was performed after extraction of analyte from vaccine media by ethyl acetate. The validity of the method was studied with a linearity of r2 &gt; 0.99 over the concentration range of 0.2–20 μg/mL with the limit of detection and the limit of quantification of 0.07 and 0.20 μg/mL, respectively. The target analyte β-propiolactone was not detected in the samples, demonstrating the test samples were qualified. The established method can be used for quality control of inactivated Covid-19 vaccines.","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.3,"publicationDate":"2024-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142264533","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":"https://doi.org/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":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-09-06","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}
Anna Ioutsi, Anastasia Sarnitskaya, Mikhail Sumtsov
{"title":"Simultaneous Determination of General Active Ingredients in Topical Formulations by Gas Chromatography with Flame Ionization Detection (GC-FID).","authors":"Anna Ioutsi, Anastasia Sarnitskaya, Mikhail Sumtsov","doi":"10.1093/chromsci/bmad086","DOIUrl":"10.1093/chromsci/bmad086","url":null,"abstract":"<p><p>A simple, fast, precision and sensitive gas chromatographic method was developed for determination of camphor, L-menthol, methyl salicylate, salicylic acid, benzyl nicotinate and nonivamide in topical formulations. The possibility of determination low-boiling components and high-boiling components by a single analytical method was shown. The method was optimized by evaluating the effect of a large number of chromatographic parameters and sample preparation stages. It was validated according to the International Council on Harmonization guidelines. Limit of quantification of active components were achieved from 0.7 μg/mL for benzyl nicotinate and L-menthol to 41 μg/mL for salicylic acid. High repeatability and good recovery values were demonstrated. The practical application of the proposed method was shown for ointments and cream.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"107591426","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":"Simultaneous Quantification of Vancomycin, Linezolid and Voriconazole in Human Plasma by UHPLC-MS/MS: Application in Therapeutic Drug Monitoring.","authors":"Yao Liu, Yanan Li, Wenli Chen, Dandan Ming, Wenji Luo, Jiabi Liang","doi":"10.1093/chromsci/bmae017","DOIUrl":"10.1093/chromsci/bmae017","url":null,"abstract":"<p><strong>Objective: </strong>Individual differences challenge the treatment of vancomycin, linezolid and voriconazole in severe infections. This study aimed to build a simple and economical method for simultaneous determination of the three antibiotics in human plasma by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and provided a reference for therapeutic drug monitoring (TDM) of infected patients.</p><p><strong>Methods: </strong>The plasma samples were precipitated by acetonitrile and detected and separated on a shim-pack GIST C18 column following the gradient elution within 5 min. Mass quantification was performed on multiple reaction monitoring mode under positive electrospray ionization.</p><p><strong>Results: </strong>The linear ranges of vancomycin, linezolid and voriconazole were 1.00-100.00, 0.10-15.00 and 0.10-20.00 μg·mL-1, respectively, with good linearity (R2 > 0.99). The accuracy and precision, matrix effect, extraction recovery and stability were validated, and the results all meet the acceptance criteria of China Food and Drug Administration (CFDA) guidelines.</p><p><strong>Conclusion: </strong>The UHPLC-MS/MS method was established and validated for the simultaneous determination of vancomycin, linezolid and voriconazole in human plasma and successfully applied to routine TDM for individualized treatment.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140898504","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":"Effects of Different Storage Times on the Stability of 12 Traditional Chinese Medicine Decoction Pieces.","authors":"Rui-Fang Xie, Yi-Ming Feng, Shan-Ni Li, Wei-Song Kong, Gui Zhou, Xin Zhou","doi":"10.1093/chromsci/bmae030","DOIUrl":"10.1093/chromsci/bmae030","url":null,"abstract":"<p><p>As storage time increases, the quality of traditional Chinese medicines (TCMs) may change, and stability is an essential aspect of ensuring the safety and efficacy of TCMs. In this study, the effects of different storage times on the stability of 12 decoction pieces were evaluated. High-performance liquid chromatography was used to determine the contents of the active components in the 12 decoction pieces. The chemical composition data were analyzed using fingerprinting and clustering heatmap (CH). Results showed that during storage, significant variations (relative standard deviation > 10%) were observed in the levels of paeoniflorin in Paeoniae Radix Alba and Paeoniae Radix Rubra, hesperidin in Citri Reticulatae Pericarpium and Citri Reticulatae Pericarpium Viride, bufothionine in Siccus Bufo and chlorogenic acid in White Chrysanthemi Flos and Lonice Raejaponicae Caulis. However, calycosin-7-glucoside and calycosin in Astragali Radix Praeparata Cum Melle and chlorogenic acid in Lonicerae Japonicae Flos, Yellow Chrysanthemi Flos and Mori Folium were all <10%, which is consistent with the CH. Decoction pieces can be stored for up to six months, but it is recommended that volatile oil-containing and animal-based decoction pieces should not be stored for more than one month. This study provides new perspectives for the stability and quality control studies of TCM.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140945047","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}
Lanyi Huang, Qing Liu, Wenfang Zhang, Bishan Lin, Yongjian Gao, Hong Deng, Shu Zhang
{"title":"Comprehensive Quality Evaluation of Danggui-Jianzhong Decoction by Fingerprint Analysis, Multi-Component Quantitation and UPLC-Q-TOF-MS.","authors":"Lanyi Huang, Qing Liu, Wenfang Zhang, Bishan Lin, Yongjian Gao, Hong Deng, Shu Zhang","doi":"10.1093/chromsci/bmae034","DOIUrl":"10.1093/chromsci/bmae034","url":null,"abstract":"<p><p>Danggui-Jianzhong decoction (DGJZ) is a famous classical traditional Chinese medicine formula, which ingredients are complex and the quality is difficult to control. Our study aimed to identify the overall chemical profile of DGJZ qualitatively by ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and UPLC. A total of 77 components, including terpenoids, flavonoids, phenolic acids, gingerols and other components, were firstly detected and characterized by UPLC-Q-TOF-MS and 18 peaks marked after analyzing the UPLC fingerprint. Finally, paeoniflorin, liquiritin, ferulic acid, cinnamic acid, glycyrrhizic acid and 6-gingerol were quantified, which was validated in terms of linearity, precision, accuracy, repeatability and recovery. Taken together, the chemical constitutes of DGJZ were systematically identified and a reliable quantitative method coupled with fingerprint analysis was successfully employed for evaluating the holistic quality, which will provide a robust foundation for the quality control of DGJZ.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141179597","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":"LC and LC-MS/MS Studies for the Separation and Identification of Impurities and Degradation Products of Betaxolol.","authors":"Anis Chmangui, Mehdi Safta, Mohamed Ridha Driss, Soufiane Touil, Sondes Bouabdallah","doi":"10.1093/chromsci/bmae025","DOIUrl":"10.1093/chromsci/bmae025","url":null,"abstract":"<p><p>Betaxolol (Bx) is a selective β1 receptor blocker used in the treatment of hypertension and glaucoma. The aim of the present work was to demonstrate an approach involving use of liquid chromatography (LC) and liquid chromatography-electrospray ionization mass spectrometry (LC-ESI/MS) for the simultaneous separation, identification and characterization of impurities and of degradation products of betaxolol without their isolation from the reaction mixtures. At optimum condition, and according to ICH guidelines, the limit of detection (LOD) and limit of quantification (LOQ) for Bx are found to be 5.46 and 16.54 μg mL-1, respectively. However, the LOD and LOQ for the major degradation product P6 were 2.15 and 6.53 μg mL-1. Betaxolol was subjected to hydrolytic (acidic and basic) and oxidative, stress conditions according to International Conference on Harmonization (ICH) guideline Q1A (R2), and as results, the drug was found to be labile in acidic, basic and oxidative stress conditions. Based on LC-ESI/MS analysis, the found results revealed that Bx decomposes in acidic, basic and oxidizing environments. All degradation products were identified with the help of their fragmentation pattern and the masses obtained upon the MS analysis.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140876569","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 Validated Chiral Chromatography Method for Enantiomeric Separation of Pomalidomide in Human Plasma.","authors":"Gyan Vardhan, Vikas Kumar, Puran Lal Sahu, Anuj Prakash, Ramasare Prasad, Shailendra Handu, Uttam Kumar Nath, Puneet Dhamija","doi":"10.1093/chromsci/bmae026","DOIUrl":"10.1093/chromsci/bmae026","url":null,"abstract":"<p><p>In the present work, new chiral stationary phase high-performance liquid chromatography (CSP-HPLC) method was established and validated for the quantification of pomalidomide (PMD) enantiomers in human plasma. The chromatographic enantiomeric separation was achieved on a Daicel-CSP, Chiralpack IA 4.6 × 250 mm, 5 μm; because of its advantages of high degree of retention, high resolution capacity, better reproducibility, ability to produce lower back pressure and low degree of tailing. The mobile phase was maintained as methanol: glacial acetic acid (499.50 ml:50 μL). Ultraviolet wavelength for detection was 220 nm. PMD enantiomer-I and enantiomer-II were separated at 8.83 and 15.34 min, respectively. Limit of detection and limit of quantification for each enantiomer and the calibration curve of standard PMD was linear in range between 10-5,000 ng mL-1. The method was validated according to The International Council for Harmonisation of Technical Requirements of Pharmaceuticals for Human Use (ICH(Q2R1)) specific guidelines. We found no interference peak with PMD chromatogram obtained. This is a simple, reliable and specific method for detection and quantification of enantiomer of PMD in human plasma sample.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140922238","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}