Analytical Chemistry Letters最新文献_第9页

Development and Validation of Rapid, Timesaving, and Cost-effective UHPLC Method for Simultaneous Quantification of Cinnarizine, its Five Specified Impurities, Two Degradation Products and Two Antioxidants 快速、省时、高效液相色谱法同时定量肉桂碱及其五种指定杂质、两种降解产物和两种抗氧化剂的建立和验证

Analytical Chemistry Letters Pub Date : 2022-07-04 DOI: 10.1080/22297928.2022.2108721

D. Mhaske, A. Kumbhar

{"title":"Development and Validation of Rapid, Timesaving, and Cost-effective UHPLC Method for Simultaneous Quantification of Cinnarizine, its Five Specified Impurities, Two Degradation Products and Two Antioxidants","authors":"D. Mhaske, A. Kumbhar","doi":"10.1080/22297928.2022.2108721","DOIUrl":"https://doi.org/10.1080/22297928.2022.2108721","url":null,"abstract":"Abstract This article explains the developed and validated rapid, timesaving, and cost-effective UHPLC method for simultaneous quantification of cinnarizine, its five specified impurities (Impurity-A to E), two degradation products (cinnamyl piperazine and benzhydrol), and two antioxidants (methylparaben and propylparaben). Furthermore, when coupled with a mass spectrometer, the proposed method provides additional advantages for confirmation of results and correct identification based on molecular weight. All analytes were eluted within 15 minutes on an ACQUITY, UPLC, BEH C18 (150 mm x 2.1 mm, 1.7 µm) column at 40.0°C by using two mobile phases containing different compositions of 10 mM ammonium acetate, acetonitrile, and acetic acid in gradient elution mode. The linearity curves of cinnarizine, its impurities, and degradation products showed good results in a correlation coefficient of 0.999 with a lower detection limit (0.1125 μg/ mL) and quantification limit (0.1875 μg/mL) at 230 nm. A forced degradation study on spiked and unspiked solutions proved their specificity with improvements and their significance. This proposed method involves a lower flow rate (0.35 mL/min.) with a shorter run time, which provides faster analysis, reduces wastage, reduces the cost, and specifies the greener advantages. The outcome of the validation as per ICH guidelines proved that the proposed UHPLC method is accurate, precise, and timesaving for simultaneous quantification of all analytes in active pharmaceutical ingredient, tablets, capsules, and oral suspension of cinnarizine. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"35 1","pages":"488 - 504"},"PeriodicalIF":0.0,"publicationDate":"2022-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72684520","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}

引用次数: 2

Determination of Impurities in Graphite Using Proton Induced Gamma Ray Emission, Total Reflection X-ray Fluorescence and Instrumental Neutron Activation Analysis 用质子诱导伽马射线发射、全反射x射线荧光和仪器中子活化分析测定石墨中的杂质

Analytical Chemistry Letters Pub Date : 2022-07-04 DOI: 10.1080/22297928.2022.2108722

M. Ghosh, T. Chavan, G. Reddy, Remya Devi P.S, S. Kumar, K. K. Swain

{"title":"Determination of Impurities in Graphite Using Proton Induced Gamma Ray Emission, Total Reflection X-ray Fluorescence and Instrumental Neutron Activation Analysis","authors":"M. Ghosh, T. Chavan, G. Reddy, Remya Devi P.S, S. Kumar, K. K. Swain","doi":"10.1080/22297928.2022.2108722","DOIUrl":"https://doi.org/10.1080/22297928.2022.2108722","url":null,"abstract":"Abstract Determination of impurities in graphite is very important for its quality control, as their presence even at trace level can affect the performance of graphite in various applications. Graphite with equivalent boron content (EBC) less than 5 mg kg-1 is considered as nuclear grade. Elements with high neutron absorption cross section (boron and rare earths) contribute significantly to EBC. Non-destructive method is preferred as there is no sample processing and probability of loss of volatile elements while digestion. Proton Induced Gamma Ray Emission (PIGE), Instrumental Neutron Activation Analysis (INAA) were utilized for the non-destructive determination of impurities in both nuclear and commercial grade graphite. Low Z elements like Li, B, F, Na, Al and Si were detected in graphite by PIGE whereas Na, K, Sc, Cr, Mn, Fe, Co, Zn, Rb, Zr, Sb, Cs, La, Ce, Nd, Sm, Eu, Tb, Yb, Hf, Ta, Th were determined using INAA. Few elements like Ca, Ti, V, Ni, Sr and Pb remained undetected by both the non-destructive techniques. These elements were determined by Total Reflection X-ray Fluorescence (TXRF) after digestion of the graphite samples by dry ashing. Combinations of these techniques were utilized to get maximum information regarding the impurities present in graphite. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"25 1","pages":"437 - 450"},"PeriodicalIF":0.0,"publicationDate":"2022-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74259766","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}

引用次数: 0

Detection of Heavy Metal Contaminants in Water and the Environment 水和环境中重金属污染物的检测

Analytical Chemistry Letters Pub Date : 2022-07-04 DOI: 10.1080/22297928.2022.2098815

P. Hitaishi, R. Verma, P. Khurana, S. Thatai

引用次数: 0

Metabolic Profiling of Averrhoa carambola Fruit Extract using UHPLC-ESI-QTOF-MS and Determination of the Concentration of Essential Elements using MP-AES 用UHPLC-ESI-QTOF-MS分析杨桃果实提取物的代谢特征，用MP-AES测定其必需元素的浓度

Analytical Chemistry Letters Pub Date : 2022-07-04 DOI: 10.1080/22297928.2022.2124125

R. Biswal, D. Patnana, V. N. R. K. Vutukuri

{"title":"Metabolic Profiling of Averrhoa carambola Fruit Extract using UHPLC-ESI-QTOF-MS and Determination of the Concentration of Essential Elements using MP-AES","authors":"R. Biswal, D. Patnana, V. N. R. K. Vutukuri","doi":"10.1080/22297928.2022.2124125","DOIUrl":"https://doi.org/10.1080/22297928.2022.2124125","url":null,"abstract":"Abstract A rapid and sensitive ultra-high-performance liquid chromatography-electrospray ionization quadrupole time of flight mass spectrometry (UHPLC-ESI-QTOF-MS) based method was developed to separate and identify 44 phenolics and non-phenolics present in Averrhoa carambola fruit in three different stages of its growth. 5 anthocyanins, 9 phenolic acids, 3 flavones, 5 flavanols, 3 flavanones, amino acids, vitamins and other phenolic and non-phenolic compounds were identified. The identification and quantification of 27 bioactive compounds from methanolic star fruit extract are being reported for the first time. All the metabolites were quantified by normalizing the area under the peaks with that of the internal standard hydrocortisone. The extraction of metabolites by using a homogeniser (bead beater) was found to be the best method for the extraction of metabolites. Four essential microelements (Zn, Fe, Mn, Cr) and three macroelements (K, Mg, Na) were quantified from star fruit using MP-AES. The zinc concentration (6.988 mg/100 g) in star fruit was found to be higher than in many cereals, vegetables and fruits. The methanolic star fruit extract showed excellent DPPH scavenging activity of 93% after 30 min of incubation in dark for the dry weight sample concentration of 50 mg/ml. In conclusion, the UHPLC-ESI-QTOF-MS based method developed and MP-AES results presented here can be used in the quality control of food supplements and medicines. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"1 1","pages":"505 - 527"},"PeriodicalIF":0.0,"publicationDate":"2022-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89312629","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}

引用次数: 0

Synchronous Fluorescence Method for Determination of Bevacizumab and Fluorouracil in Laboratory Prepared Mixture, Pharmaceutical Dosage Forms and Spiked Plasma 同步荧光法测定实验室制剂、制剂和加标血浆中贝伐单抗和氟尿嘧啶的含量

Analytical Chemistry Letters Pub Date : 2022-07-04 DOI: 10.1080/22297928.2022.2088300

H. Salem, Mohamed A. Mawhoup, M. Sayed, A. Abdelaziz

{"title":"Synchronous Fluorescence Method for Determination of Bevacizumab and Fluorouracil in Laboratory Prepared Mixture, Pharmaceutical Dosage Forms and Spiked Plasma","authors":"H. Salem, Mohamed A. Mawhoup, M. Sayed, A. Abdelaziz","doi":"10.1080/22297928.2022.2088300","DOIUrl":"https://doi.org/10.1080/22297928.2022.2088300","url":null,"abstract":"Abstract Bevacizumab (BVC) is commonly co-administered with 5-fluorouracil (FLO) as a highly successful treatment for colon cancer. In this study, two spectrofluorimetric techniques were combined to provide an approach for concurrent quantification of BVC and FLO that is very sensitive, quick, easy and accurate. The inclusion of Tween-80 micellar system increased the native fluorescence intensity values of BVC and FLO, while the second derivative of the synchronous fluorescence intensity of the cited drugs at Δλ=100 nm allowed the concurrent estimation of cited drugs. The effect of various experimental conditions on the synchronous fluorescence of cited drugs were extensively examined to optimize them. The second derivative synchronous fluorimetry peak amplitudes for BVC and FLO were recorded at 450 nm and 440 nm, respectively. At a range of 100–1100 and 100–600 ng mL−1, the fluorescence-concentration graphs were built, with smaller quantification limits of 60.0 and 70.0 ng mL−1 and detection limits of 20.0 and 23.0 ng mL−1 for BVC and FLO, respectively. Without any major interference, the technique was effectively used to determine the cited drugs in raw material along with pharmaceutical formulations. The proposed technique was shown to be extremely precise and accurate when related to the reported techniques statistically. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"194 2","pages":"460 - 472"},"PeriodicalIF":0.0,"publicationDate":"2022-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91503480","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}

引用次数: 1

The Use of Liquid Chromatography and Mass Spectrometry to Identify and Quantify Chemical Components in Tea Extracts 用液相色谱和质谱法鉴定和定量茶叶提取物中的化学成分

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2088299

Diavian Bellamy, Mieka Cobbs, S. Rahhal, A. Bakarr Kanu

{"title":"The Use of Liquid Chromatography and Mass Spectrometry to Identify and Quantify Chemical Components in Tea Extracts","authors":"Diavian Bellamy, Mieka Cobbs, S. Rahhal, A. Bakarr Kanu","doi":"10.1080/22297928.2022.2088299","DOIUrl":"https://doi.org/10.1080/22297928.2022.2088299","url":null,"abstract":"Abstract A fast, straightforward, efficient, and high throughput reverse-phase high-performance liquid chromatography and electrospray ionization mass spectrometry method has been developed to analyze tea extracts containing polyphenols. The polyphenols detected in green tea (GT), black tea (BT), and paradise tropical tea (PTT) were separated in 18 min at wavelengths 254 nm, 260 nm, and 280 nm with a gradient elution on the RP-HPLC system. Our approach detected, identified, and quantified three catechins in the tea extracts analyzed, and the response at 280 nm wavelength was the best. The ESI-MS data confirmed the fragmentation patterns of the catechins detected in the tea extract. The validation data showed that the limit of detection (LOD) and limit of quantitation (LOQ) of catechins ranged from 5.26 ± 0.02 to 36.44 ± 0.02 ppb, and 17.52 ± 0.03 to 121.45 ± 0.16 ppb, respectively, for six catechins studied. The standard addition calibration approach used to quantify the catechin content in the tea extract simultaneously showed that PTT has a higher catechin content than GT and BT. The content of polyphenols in GT, BT, and PTT are summarized. This approach holds great promise for quality control studies to quantify polyphenols in nutritional products. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"431 1","pages":"292 - 301"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76660489","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}

引用次数: 1

Development and Validation of a New Stereoselective RP-HPLC Method for Simultaneous Quantification of Tadalafil, its One Enantiomer, and Two Diastereomers in API and Tablet Form 同时定量他达拉非原料药和片剂中1个对映体和2个非对映体的新立体选择性RP-HPLC方法的建立和验证

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2089595

D. Mhaske, A. Kumbhar

{"title":"Development and Validation of a New Stereoselective RP-HPLC Method for Simultaneous Quantification of Tadalafil, its One Enantiomer, and Two Diastereomers in API and Tablet Form","authors":"D. Mhaske, A. Kumbhar","doi":"10.1080/22297928.2022.2089595","DOIUrl":"https://doi.org/10.1080/22297928.2022.2089595","url":null,"abstract":"Abstract A new, simple, and stereoselective RP-HPLC method was developed and validated for the simultaneous quantification of tadalafil, its one enantiomer, and two diastereomers in API and tablets. Using varied compositions of water, acetonitrile, and acetic acid as mobile phases in gradient mode at a 0.40 mL/min flow rate and detection at 285 nm, all this separation was achieved on the Lux Cellulose-3 (150 mm x 4.6 mm, 3 µm) column at a 30.0°C oven temperature. All isomers were eluted within 24 minutes, with a resolution of more than 2.3 between any two isomers. With 10.0 µL injection volume, the LOD and LOQ were determined to be 0.06 µg/mL and 0.10 µg/mL, respectively. The linearity of tadalafil (0.10-400 µg/mL), one enantiomer, and two diastereomers (0.10-4.0 µg/mL) was confirmed with a correlation coefficient of 0.999. The forced degradation study revealed the specificity for all the peaks as well as the conversion of tadalafil into diastereomers (6S, 12aR) in acidic conditions and into diastereomers (6R, 12aS) in alkaline conditions. At lower concentrations, the recoveries for all isomers ranged from 100.0 ± 15.0%, while the assay values for tadalafil were within 100.0 ± 2.0%. According to the validation outcome as per ICH guidelines, the proposed method is an accurate, precise, linear, and robust stereoselective method for simultaneous quantification. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"5 1","pages":"419 - 436"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75227148","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}

引用次数: 0

The New RP-HPLC Method for Simultaneous Quantification of Cinnarizine, its Five Specified Impurities, Two Degradation Products with Two Antioxidants and Confirmation of all by HPLC-ESI-MS in Different Pharmaceutical Drug Formulations 采用反相高效液相色谱(RP-HPLC)同时定量测定不同制剂中肉桂碱、五种指定杂质、两种抗氧化剂降解产物，并采用HPLC-ESI-MS确认

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2067006

D. Mhaske, A. Kumbhar

{"title":"The New RP-HPLC Method for Simultaneous Quantification of Cinnarizine, its Five Specified Impurities, Two Degradation Products with Two Antioxidants and Confirmation of all by HPLC-ESI-MS in Different Pharmaceutical Drug Formulations","authors":"D. Mhaske, A. Kumbhar","doi":"10.1080/22297928.2022.2067006","DOIUrl":"https://doi.org/10.1080/22297928.2022.2067006","url":null,"abstract":"Abstract To determine the safety and efficacy, we have developed and validated the RP-HPLC method for simultaneous quantification of cinnarizine, its five specified impurities and two degradation products in cinnarizine API, tablets and capsules and including two antioxidants in an oral suspension formulation. The chromatographic separation was achieved in gradient elution mode with 1.00mL/min flow on an Ascentis Express C18 (150mm, 4.6mm and 2.7µm particle size) column at 40.0°C column temperature using 0.05% acetic acid in mixtures of 10mM ammonium acetate and acetonitrile. All peaks are eluted within 30 minutes with a 10µL injection volume and detected at a 230nm wavelength. The results of the validation of the proposed RP-HPLC method as per ICH guidelines revealed that the method is specific, accurate, precise, linear and robust for quantification purposes. The recoveries for all specified impurities, degradation products and cinnarizine at a lower concentration were found in the range of 100.0±10.0%. While the assay values were within 100.0±2.0% for cinnarizine and antioxidants (methylparaben and propylparaben). The LOD and LOQ were 0.1125µg/mL and 0.1875µg/mL, respectively. The linearity curves for all the ten analytes mentioned above showed good linearity (r≥0.999). This research work presents the first RP-HPLC method for simultaneous quantification of all ten analytes with unknown impurities, as well as an HPLC-ESI-MS method for correct identification and confirmation of results. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"8 1","pages":"391 - 408"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84235504","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}

引用次数: 1

Resolving Problems Encountered in Spectrophotometric Analysis of a Ternary Mixture of Linagliptin, Empagliflozin and Metformin Hydrochloride 利格列汀、恩格列净、盐酸二甲双胍三元混合物分光光度法分析中存在的问题

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2058414

Samar H. Elagamy

{"title":"Resolving Problems Encountered in Spectrophotometric Analysis of a Ternary Mixture of Linagliptin, Empagliflozin and Metformin Hydrochloride","authors":"Samar H. Elagamy","doi":"10.1080/22297928.2022.2058414","DOIUrl":"https://doi.org/10.1080/22297928.2022.2058414","url":null,"abstract":"Abstract There are two main problems encountered in spectrophotometric analysis of a ternary mixture composed of linagliptin LINA, empagliflozin EMPA and metformin hydrochloride MET. The first problem is due to the severe overlap in their zero and derivative spectra. To overcome this problem, LINA was determined by direct spectrophotometry at λ max = 298 nm where there is no interference from other components while, EMPA and MET were determined using double divisor ratio spectra derivative method DDRD. In this method, the first derivative spectra were calculated for ratio spectra generated by dividing the absorption spectra of ternary mixtures containing increasing concentrations of one of the components by a standard spectrum of binary mixture of the other two components (double divisor). The calibration graphs were constructed by measuring the amplitude at either the minimum or maximum wavelengths against the concentrations. The selected wavelengths for determination of EMPA and MET are 282.92 and 250 nm, respectively. The second problem arises from the presence of LINA and EMPA as minor components in their recently approved dosage form with MET thus, sample enrichment through spiking was employed for LINA and EMPA to enable their spectrophotometric analysis in laboratory prepared mixtures that have the same ratio of the three components as in their pharmaceutical dosage form. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"20 1","pages":"349 - 357"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77736689","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}

引用次数: 1

PEG-400 Catalyzed N-C, O-C & C-S Bond Formations: A Robust Sonication Promoted Synthesis of Benzo[d]oxazole-2 (3H)-thione & Benzo[d]thiazole-2(3H)-thione Hybrids PEG-400催化的N-C, O-C和C-S键形成:一个稳健的超声催化合成苯并[d]恶唑-2(3H)-硫酮和苯并[d]噻唑-2(3H)-硫酮杂化物

Analytical Chemistry Letters Pub Date : 2022-05-04 DOI: 10.1080/22297928.2022.2068376

Aadil Yaseen, M. Waseem, Mahapara Qadir, P. Dar, Shariqah Hijazi, Mir Ashiq Hussain, W. A. Shah

引用次数: 0