{"title":"Single Method for Determination of Biocides Benzalkonium Chloride, Chloroxylenol and Chlorhexidine Gluconate in Cosmetics, Hygiene and Health Care Products by Using High Performance Liquid Chromatography.","authors":"Kumar Thangarathinam, Meenakshi Narayanan, Ashwin Kumar Ks, Banupriya Arjunan, Divya Bhavani Raja","doi":"10.1093/chromsci/bmae039","DOIUrl":"10.1093/chromsci/bmae039","url":null,"abstract":"<p><p>Benzalkonium chloride (BKC), chloroxylenol (PCMX) and chlorhexidine gluconate (CHG) are widely recognized biocidal compounds that require precise control and monitoring in various applications, including cosmetics, hygiene, health and ophthalmic products. In this study, we present a straightforward and highly sensitive high-performance liquid chromatographic (HPLC) method for the detection of these substances. The HPLC method we developed allows for the detection of BKC at concentrations as low as 1.0 ppm, PCMX at 1.0 ppm and CHG at 2.0 ppm, all with a signal-to-noise (S/N) ratio exceeding 3.0. Additionally, the method enables quantification up to 2.0 ppm for BKC, 2.0 ppm for PCMX and 5 ppm for CHG, with an S/N ratio surpassing 10.0. This validated method serves as a versatile tool for the accurate quantification of BKC, PCMX and CHG in cosmetics, hygiene products, health products and ophthalmic products. Its applicability extends across a wide range of industries, ensuring the reliable assessment of these critical biocides.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"837-844"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141293419","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}
Lixin Song, Jian Zhang, Mingyu Wang, Zhipeng Huang, Yunxia Zhang, Xing Zhang, Yutao Liang, Juan He
{"title":"Simultaneously Selective Separation of Zearalenone and Four Aflatoxins From Rice Samples Using Co-Pseudo-Template Imprinted Polymers With MIL-101(Cr)-NH2 as Core.","authors":"Lixin Song, Jian Zhang, Mingyu Wang, Zhipeng Huang, Yunxia Zhang, Xing Zhang, Yutao Liang, Juan He","doi":"10.1093/chromsci/bmae041","DOIUrl":"10.1093/chromsci/bmae041","url":null,"abstract":"<p><p>A novel approach for the simultaneous separation of zearalenone (ZEN) and four types of aflatoxins (AFB1, AFB2, AFG1 and AFG2) from rice samples was presented. This approach utilized modified MIL-101(Cr)-NH2 as core, with molecularly imprinted polymers (MIPs) serving as the shell. The MIL-101(Cr)-NH2 was prepared via ring-opening reaction, while the imprinted polymers were synthesized using warfarin and 4-methylumbelliferyl acetate as co-pseudo template, ethylene glycol dimethacrylate as the cross-linker and azobisisobutyronitrile as initiator. The resulting co-pseudo-template-MIPs (CPT-MIPs) were thoroughly characterized and evaluated. Adsorption studies demonstrate that the adsorption process of CPT-MIPs follows a chemical monolayer adsorption mechanism, with imprinted factors ranging from 1.24 to 1.52 and selective factors ranging from 1.29 to 1.52. Self-made columns were prepared, and the method for separation was developed and validated. The limit of detections ranged from 0.12 to 2.09 μg/kg, and the limit of qualifications ranged from 1.2 to 6.25 μg/kg. To assess the reliability of the method, ZEN and AFs were spiked at three different levels, and the recoveries ranged from 79.53 to 94.58%, with relative standard deviations of 2.90-5.78%.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"892-903"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141306047","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":"HPTLC Method Development and Validation for the Simultaneous Estimation of Nortriptyline HCl and Pregabalin in their Combined Dosage Form.","authors":"Hinal Harkhani, Kashyap Thummar, Sanjay Chauhan, Jigna Vadalia","doi":"10.1093/chromsci/bmad081","DOIUrl":"10.1093/chromsci/bmad081","url":null,"abstract":"<p><p>Nortriptyline HCl and pregabalin Tablet is used to treat neuropathic pain as well as mental or mood issues such as sadness, mood, feelings, anxiety and tensions. Very few analytical methods are available for the simultaneous estimation of nortriptyline HCl and pregabalin and no reports has been found for HPTLC method. In the current study, a reliable HPTLC method for the simultaneous measurement of nortriptyline HCl and pregabalin in pure forms and pharmaceutical formulations has been developed with ninhydrine post derivatization of pregabalin. The HPTLC method development was carried using silica gel G60 F254 as stationary phase and acetonitrile: methanol: triethylamine: water: formic acid (7:3:0.3:0.8:0.02 v/v/v/v/v) was used as mobile phase with saturation time of 20 min. The system was found to give a compact band for nortriptyline HCl (Rf = 0.523 ± 0.008) pregabalin (Rf = 0.279 ± 0.005). The developed method was found to be validated as per ICH Q2 (R1) guideline. The peak of nortriptyline HCl and pregabalin showed good linearity over the concentration range of 50-300 ng/band and 350-2250 ng/band, respectively, with a correlation coefficient of ˃0.995. The % recoveries of both drugs were found to be in the range of 98.84-101.87%. Statistical analysis proved that the method is selective, precise, robust and accurate for the estimation of nortriptyline HCl and pregabalin.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"886-891"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49677964","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}
Fatma F Abdallah, M Fatma, Ahmed M Gouda, Eglal A Abdelaleem, Aml A Emam
{"title":"Ecofriendly HPLC Method for Simultaneous Determination of the Co-Prescribed Drugs in Chemotherapy Omeprazole, Ondansetron and Deflazacort in Spiked Human Plasma.","authors":"Fatma F Abdallah, M Fatma, Ahmed M Gouda, Eglal A Abdelaleem, Aml A Emam","doi":"10.1093/chromsci/bmad088","DOIUrl":"10.1093/chromsci/bmad088","url":null,"abstract":"<p><p>Green, selective and accurate high-performance liquid chromatography (HPLC) chromatographic method is presented for simultaneous separation and quantitation of the co-prescribed drugs in chemotherapy omeprazole, ondansetron and deflazacort in spiked human plasma. An isocratic HPLC separation was performed on X Bridge C18 (4.6 × 250 mm) column with 5 μm particle size using mobile phase consisting of methanol: ammonium acetate buffer pH 4 adjusted by acetic acid (60: 40, v/v). The injection volume was 20μL with UV detection wavelength at 237 nm at room temperature. Flow rate of the mobile phase was adjusted to be 2.0 ml/min. Dexamethasone was used as internal standard to correct the variation during sample pretreatment. FDA guidelines were followed to validate the developed method. Successful application of the developed method was revealed by simultaneous determination of omeprazole, ondansetron and deflazacort in spiked human plasma in ranges of 1-20, 0.1-8 and 0.2-8 μg mL-1 for omeprazole, ondansetron and deflazacort, respectively. Four greenness assessment tools were used to evaluate the greenness of the developed method and the results were accepted. This method permitted the accurate simultaneous determination of the studied drugs, thus it can be used during therapeutic drug monitoring in daily clinical practice.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"845-853"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138299185","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}
Pablo Miranda, Analía Castro, Luisina Rodríguez Grassi, Danilo Davyt, Marcelo Hill, Mercedes Segovia, Alvaro W Mombrú, Helena Pardo
{"title":"Reverse Phase HPLC Methodology for the Determination of Bay K8644.","authors":"Pablo Miranda, Analía Castro, Luisina Rodríguez Grassi, Danilo Davyt, Marcelo Hill, Mercedes Segovia, Alvaro W Mombrú, Helena Pardo","doi":"10.1093/chromsci/bmae011","DOIUrl":"10.1093/chromsci/bmae011","url":null,"abstract":"<p><p>Following ICH guidelines for analytical validation, we report a common C18 column stability indicating isocratic reverse phase high performance liquid chromatography method for the determination of the ion channel modulator Bay K8644. Two main forced degradation products and a minor impurity were also tentatively identified by Mass Spectrometry. The mobile phase consisted of a 50/50 acetonitrile/buffer mixture at a flow rate of 2 mL/min. Mean retention time for Bay K8644 was 3.030 minutes. Excellent linearity (r = 0.9998) was achieved in the range 0.10-1.40 μg/mL at 274 nm wavelength. Analytical limits were 16.56 ± 1.04 ng/mL for detection and 55.21 ± 3.48 ng/mL for quantitation respectively. Accuracy and precision studies showed good results (95-105%). Robustness was assessed by varying ±3%, both temperature and flow rate. Five different stress conditions were applied to assess Bay K8644's stability. Only basic and photolytic treatments yielded degradation products, both correctly resolved in a total runtime of 4 minutes. In conclusion, we developed a fast, simple, sensitive, accurate, precise, reliable and stability indicating method for detecting/quantifying Bay K8644, and tentatively characterized its main impurities/forced degradation products.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"829-836"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140326636","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}
Ola G Hussein, Yasmin Rostom, Mohamed Abdelkawy, Mamdouh R Rezk, Dina A Ahmed
{"title":"Green TLC-Densitometric Method for Simultaneous Determination of Antazoline and Tetryzoline: Application to Pharmaceutical Formulation and Rabbit Aqueous Humor.","authors":"Ola G Hussein, Yasmin Rostom, Mohamed Abdelkawy, Mamdouh R Rezk, Dina A Ahmed","doi":"10.1093/chromsci/bmad042","DOIUrl":"10.1093/chromsci/bmad042","url":null,"abstract":"<p><p>Ophthalmic pharmaceutical preparation containing antazoline (ANT) and tetryzoline (TET) is prescribed widely as an over the counter medication for allergic conjunctivitis treatment. Development of a selective, simple and environmentally friendly thin-layer chromatographic method established to determine both ANT and TET in their pure forms, pharmaceutical formulation and spiked aqueous humor samples. By using silica gel plates and means of a developing system consists of ethyl acetate:ethanol (5:5, by volume), the studied drugs separation was achieved, and scanning was carried out at 220.0 nm for the separated bands with a 0.2-18.0 μg/band concentration range for each of ANT and TET. Standard addition technique application was carried out to determine the proposed method validity. Statistical comparison was made between the proposed method and the official methods ANT and TET showing no significant difference concerning accuracy and precision. Furthermore, greenness profile assessment was accomplished by means of four metric tools, namely, analytical greenness, green analytical procedure index, analytical eco-scale and national environmental method index.</p><p><p>Highlights.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"807-814"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9988749","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":"Development and Validation of a SPE-HPLC Method for Quantification of Rhein, Emodin, Chrysophanol and Physcion in Rhamnus petiolaris Boiss. & Balansa.","authors":"Pelin Köseoğlu Yılmaz, Ufuk Kolak","doi":"10.1093/chromsci/bmad053","DOIUrl":"10.1093/chromsci/bmad053","url":null,"abstract":"<p><p>Anthraquinones exhibit a significant group of natural and synthetic quinone derivatives because of their biological activities and industrial applications. Rhamnaceae is one of the families known to contain different kinds of anthraquinones. In this study, it was aimed to quantify rhein, emodin, chrysophanol and physcion in fruits of Rhamnus petiolaris Boiss. & Balansa belonging to Rhamnaceae by solid phase extraction and high performance liquid chromatography with ultraviolet detection. The anthraquinones were separated using a C18 analytical column. Gradient elution was performed using a mobile phase consisted of 0.1% o-phosphoric acid solution and methanol. Analytes were detected at 254 nm. Calibration curves were prepared in the range of 0.25-5.00 μg/mL for rhein, chrysophanol, physcion, 1.00-50.00 μg/mL for emodin. Limits of detection and quantification were between 0.07-0.11 and 0.20-0.34 μg/mL, respectively. Relative standard deviations were ≤ 5.78% in repeatability and intermediate precision studies. Accuracy was determined as relative mean error (8.17-12.06%). Extraction was achieved by maceration with acetone and ethanol, followed by hydrophilic-lipophilic balance solid phase extraction. Recoveries were between 96.2 and 109.6%. The developed and validated method was successfully performed to quantify rhein, emodin, chrysophanol and physcion in R. petiolaris fruit extracts. Only physcion was not detected above limit of detection.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"872-877"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11530379/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10259909","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Development and Validation of a Simple High-Pressure Liquid Chromatography-Ultraviolet Detection Method for Simultaneous Quantitation of First-Line Anti-Tuberculosis Drugs in Formulations of Fixed-Dose Combination.","authors":"Sudha Vilvamani, Santhanamahalingam Mahalingam, Sruthi Nhavilthodi, Dharman Murugesan, Shanmugam Murugaiha Jeyakumar","doi":"10.1093/chromsci/bmae023","DOIUrl":"10.1093/chromsci/bmae023","url":null,"abstract":"<p><p>The current treatment protocol for drug-sensitive tuberculosis involves all four first-line anti-tuberculosis drugs: rifampicin, isoniazid, pyrazinamide and ethambutol hydrochloride in a single tablet, known as fixed-dose combination tablets. However, the analytical methods are scanty to test all these drugs simultaneously in a single run without any pre-sample process or using a simple method suitable for resource-limited settings. In this method, 50 mM potassium phosphate buffer containing 0.2% triethylamine (without pH adjustment) added with acetonitrile (98:2, v/v) was served as mobile phase A, while mobile phase B was 100% acetonitrile. All four drugs were separated within 10.3 min using a gradient mobile phase program in a C18 column (150 mm × 4.6 mm; 5 μm) and detected at two ultraviolet wavelengths (238 nm for rifampicin, isoniazid and pyrazinamide, and 210 nm for ethambutol hydrochloride). The method was selective, sensitive and linear with a correlation coefficient >0.999 with the acceptable precision and accuracy (<2% relative standard deviation) for all four drugs. In conclusion, the method is simple and it does not require any pH adjustment of the buffer/mobile phase, and within 11 min, the separation of all four drugs can be achieved. Overall, the method is suitable for quality testing of fixed-dose combination tablets in limited-resource settings.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"821-828"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140876568","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}
Xiaoli Xu, Lin Yang, Dezhang Zhao, Yiwu Wang, Lei Dai, Shuya Li, Dan He
{"title":"New Quality Evaluation of Qizhi Xiangfu Pills Based on Fingerprint with Chemometric Analysis and Quantitative Analysis of Multi-Components by Single Marker.","authors":"Xiaoli Xu, Lin Yang, Dezhang Zhao, Yiwu Wang, Lei Dai, Shuya Li, Dan He","doi":"10.1093/chromsci/bmae005","DOIUrl":"10.1093/chromsci/bmae005","url":null,"abstract":"<p><p>Qizhi Xiangfu Pills (QZXFPs) is one of the most commonly used traditional Chinese medicine preparations for the treatment of dysmenorrhea, 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 combined with chemometric analysis and quantitative analysis of multi-components by a single marker (QAMS) method was used to comprehensively evaluate the quality of QZXFPs. The fingerprints of 28 batches samples were established and 23 common peaks were distinguished, of which 7 peaks were identified as albiflorin, paeoniflorin, baicalin, ligustilide, cyperotundone, nootkatone and α-cyperone. The content of these seven active ingredients was determined simultaneously by the QAMS method and there was no significantly different between QAMS and the external standard method. Additionally, similarity analysis, hierarchical cluster analysis, principal component analysis and orthogonal partial least squares discrimination analysis were applied for classifying the 28 batches of samples, and to find the main components causing the quality differences between different batches. In conclusion, the established method can comprehensively evaluate the consistency of quality between different batches and provide a reference for formulation quality evaluation to ensure safe and effective application of QZXFPs.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":"854-863"},"PeriodicalIF":1.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140049658","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":"Application of Polydopamine-Based Magnetic Solid-Phase Extraction for Highly Sensitive Determination of Aristolochic Acid I from Traditional Chinese Medicine Samples.","authors":"Huimin Li, Huina Cao, Zixin Zhang, Fei Tian, Yi Zhang, Lijie Wu","doi":"10.1093/chromsci/bmae055","DOIUrl":"https://doi.org/10.1093/chromsci/bmae055","url":null,"abstract":"<p><p>A low cost-effective and simple synthesis method combining magnetic solid-phase extraction (MSPE) and high-pressure liquid chromatography was developed for the analysis of aristolochic acids I (AAI) in traditional Chinese medicine samples. A novel polydopamine (PDA) modified magnetic nanoparticles with one single carbon layer (Fe3O4@1C NPs) via one-pot hydrothermal approach was prepared and then successfully employed to extract AAI for the first time. Dopamine (DA) can form a PDA layer on Fe3O4@1C NPs surface through self-polymerization to form Fe3O4@1C@PDA. As a surface modifier of DA, PDA offered more adsorption sites to AAI due to π-π stacking, hydrogen bonding and electrostatic interactions. The parameters of MSPE were optimized by univariate and multivariate methods (Box-Behnken design) in detail. High degree of linearity was obtained in the range of 0.05-200.0 μg/mL. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.08 and 0.25 μg/mL, respectively. The recoveries of AAI in spiked Xiaoqinglong mixture samples were in the range of 86.7 to 108.5% with the relative standard deviation of less than 5.2%. Thus, a fast, convenient, sensitive and eco-friendly method was successfully proposed and became a promising approach for the determination of AAI in herbal plants or its preparation in the manufacturing procedure.</p>","PeriodicalId":15430,"journal":{"name":"Journal of chromatographic science","volume":" ","pages":""},"PeriodicalIF":1.5,"publicationDate":"2024-10-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142545731","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}