Pub Date : 2022-07-04DOI: 10.1080/22297928.2022.2108721
D. Mhaske, A. Kumbhar
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
摘要:本文建立并验证了一种快速、省时、高性价比的同时定量肉桂嗪及其5种指定杂质(杂质- a至E)、2种降解产物(肉桂基哌嗪和苯并氢)和2种抗氧化剂(对羟基苯甲酸甲酯和对羟基苯甲酸丙酯)的UHPLC方法。此外，当与质谱仪相结合时，该方法在结果的确认和基于分子量的正确鉴定方面具有额外的优势。所有分析物在ACQUITY, UPLC, BEH C18 (150 mm x 2.1 mm, 1.7µm)柱上，在40.0°C下，用两种流动相(含10 mm乙酸铵，乙腈和乙酸的不同组成)梯度洗脱，在15分钟内洗脱。肉桂碱及其杂质与降解产物的线性关系良好，相关系数为0.999，在230 nm处检出限低(0.1125 μg/mL)，定量限低(0.1875 μg/mL)。对加钉和未加钉溶液的强制降解研究证明了它们的特异性和改进的意义。该方法的流速较低(0.35 mL/min)，运行时间较短，分析速度更快，减少了浪费，降低了成本，并具有更环保的优势。根据ICH指南的验证结果证明，所提出的UHPLC方法准确，精确，节省时间，可同时定量肉桂碱的活性药物成分，片剂，胶囊和口服混悬液中的所有分析物。图形抽象
{"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}
Pub Date : 2022-07-04DOI: 10.1080/22297928.2022.2108722
M. Ghosh, T. Chavan, G. Reddy, Remya Devi P.S, S. Kumar, K. K. Swain
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
{"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}
Pub Date : 2022-07-04DOI: 10.1080/22297928.2022.2098815
P. Hitaishi, R. Verma, P. Khurana, S. Thatai
Abstract A simple and highly sensitive plasmonic colorimetric method using nanomaterials is reviewed to detect heavy metal ions in aqueous samples. The basic properties of nanomaterials, which make them behave differently from their bulk counterpart is addressed. The main focus is on the potential applications of intelligent materials like metal NPs and core-shell nanocomposites for the sensing of heavy metal ions in an aqueous media and environment. The article also presents an overview of the science and technology behind nanoparticle-based sensors in general and core-shell sensors in particular. This article embodies an overview of the exciting and emerging field of sensors with an emphasis on metal nanoparticles and core-shell nanocomposites. GRAPHICAL ABSTRACT
{"title":"Detection of Heavy Metal Contaminants in Water and the Environment","authors":"P. Hitaishi, R. Verma, P. Khurana, S. Thatai","doi":"10.1080/22297928.2022.2098815","DOIUrl":"https://doi.org/10.1080/22297928.2022.2098815","url":null,"abstract":"Abstract A simple and highly sensitive plasmonic colorimetric method using nanomaterials is reviewed to detect heavy metal ions in aqueous samples. The basic properties of nanomaterials, which make them behave differently from their bulk counterpart is addressed. The main focus is on the potential applications of intelligent materials like metal NPs and core-shell nanocomposites for the sensing of heavy metal ions in an aqueous media and environment. The article also presents an overview of the science and technology behind nanoparticle-based sensors in general and core-shell sensors in particular. This article embodies an overview of the exciting and emerging field of sensors with an emphasis on metal nanoparticles and core-shell nanocomposites. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"2017 1","pages":"473 - 487"},"PeriodicalIF":0.0,"publicationDate":"2022-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90654364","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}
Pub Date : 2022-07-04DOI: 10.1080/22297928.2022.2124125
R. Biswal, D. Patnana, V. N. R. K. Vutukuri
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
{"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}
Pub Date : 2022-07-04DOI: 10.1080/22297928.2022.2088300
H. Salem, Mohamed A. Mawhoup, M. Sayed, A. Abdelaziz
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
贝伐单抗(BVC)通常与5-氟尿嘧啶(FLO)合用，作为一种非常成功的结肠癌治疗方法。本研究将两种荧光光谱技术相结合，为BVC和FLO的同时定量提供了一种灵敏、快速、简便、准确的方法。Tween-80胶束体系的加入提高了BVC和FLO的天然荧光强度值，同时对被引药物在Δλ=100 nm处的同步荧光强度进行二阶导数，可以对被引药物进行并发估计。广泛考察了各种实验条件对被引药物同步荧光的影响，并对其进行了优化。BVC和FLO的二阶导数同步荧光峰分别在450 nm和440 nm处记录。在100-1100和100-600 ng mL−1范围内建立荧光浓度图，BVC和FLO的定量限分别为60.0和70.0 ng mL−1，检测限分别为20.0和23.0 ng mL−1。该技术在不受干扰的情况下，可有效地测定原料和制剂中的被引药物。所提出的技术被证明是极其精确和准确的，当相关的报道技术统计。图形抽象
{"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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2088299
Diavian Bellamy, Mieka Cobbs, S. Rahhal, A. Bakarr Kanu
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
{"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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2089595
D. Mhaske, A. Kumbhar
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
建立了一种新的、简单的、立体选择性的反相高效液相色谱(RP-HPLC)方法，用于同时测定原料药和片剂中他达拉非及其1个对映体和2个非对映体的含量。使用不同的水、乙腈和乙酸作为流动相，在梯度模式下，流速为0.40 mL/min，检测波长为285 nm，在30.0°C的烤箱温度下，在Lux Cellulose-3 (150 mm x 4.6 mm, 3µm)柱上实现了所有这些分离。所有异构体均在24分钟内洗脱，任意两个异构体之间的分辨率均大于2.3。在进样量为10.0µL时，定量限和定量限分别为0.06µg/mL和0.10µg/mL。他达拉非(0.10 ~ 400µg/mL)与1个对映体、2个非对映体(0.10 ~ 4.0µg/mL)的线性关系为0.999。强制降解研究揭示了所有峰的特异性，以及他达拉非在酸性条件下转化为非对映体(6S, 12aR)和在碱性条件下转化为非对映体(6R, 12aS)。在较低浓度下，各异构体的回收率为100.0±15.0%，他他拉非的测定值为100.0±2.0%。根据ICH指南的验证结果，所提出的方法是一种准确、精确、线性和稳健的立体选择性同时定量方法。图形抽象
{"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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2067006
D. Mhaske, A. Kumbhar
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
{"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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2058414
Samar H. Elagamy
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
摘要:利格列汀LINA、恩格列净EMPA和盐酸二甲双胍MET组成的三元混合物在分光光度分析中存在两个主要问题。第一个问题是由于它们的零谱和导数谱的严重重叠。为了克服这一问题，在λ max = 298 nm处，在不受其他组分干扰的情况下，采用直接分光光度法测定LINA，而采用双因子比光谱导数法测定EMPA和MET。该方法通过将含有一种组分浓度增加的三元混合物的吸收光谱除以另外两种组分的二元混合物的标准光谱(双除数)得到比值光谱的一阶导数光谱。通过测量最小或最大波长对浓度的振幅来构建校准图。选择测定EMPA和MET的波长分别为282.92 nm和250 nm。第二个问题来自LINA和EMPA作为次要成分在其最近批准的含有MET的剂型中存在，因此，LINA和EMPA采用了通过峰化的样品富集，以便在实验室制备的混合物中进行分光光度分析，这些混合物具有与药物剂型中相同的三种成分比例。图形抽象
{"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}
Pub Date : 2022-05-04DOI: 10.1080/22297928.2022.2068376
Aadil Yaseen, M. Waseem, Mahapara Qadir, P. Dar, Shariqah Hijazi, Mir Ashiq Hussain, W. A. Shah
Abstract Herein an efficient and green protocol has been disclosed for the synthesis of biologically competent and structurally simple benzo[d]oxazole-2(3H)-thione/benzo[d]thiazole-2(3H)-thione derivatives. The reaction has been carried out under sonication at 15oC up to 11 hours. Timely progress of the reaction was monitored by using TLC technique. The simple skeletal product with strong biological profile synthesized via simple reaction procedure under complete green conditions is highly useful as per environmental concerns. The unveiled methodology is highly efficient and easy handling as it is devoid of any transition metal catalyst and volatile organic solvent, mostly used for reaction progress. Further, the use of polyethylene glycol, a green catalyst, sonication a selective energy source, better product yield and feasible reaction time are supplementary attributes towards the developed methodology. GRAPHICAL ABSTRACT
{"title":"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","authors":"Aadil Yaseen, M. Waseem, Mahapara Qadir, P. Dar, Shariqah Hijazi, Mir Ashiq Hussain, W. A. Shah","doi":"10.1080/22297928.2022.2068376","DOIUrl":"https://doi.org/10.1080/22297928.2022.2068376","url":null,"abstract":"Abstract Herein an efficient and green protocol has been disclosed for the synthesis of biologically competent and structurally simple benzo[d]oxazole-2(3H)-thione/benzo[d]thiazole-2(3H)-thione derivatives. The reaction has been carried out under sonication at 15oC up to 11 hours. Timely progress of the reaction was monitored by using TLC technique. The simple skeletal product with strong biological profile synthesized via simple reaction procedure under complete green conditions is highly useful as per environmental concerns. The unveiled methodology is highly efficient and easy handling as it is devoid of any transition metal catalyst and volatile organic solvent, mostly used for reaction progress. Further, the use of polyethylene glycol, a green catalyst, sonication a selective energy source, better product yield and feasible reaction time are supplementary attributes towards the developed methodology. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"16 1","pages":"302 - 309"},"PeriodicalIF":0.0,"publicationDate":"2022-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87061241","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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