Ishita A. Basera, A. Girme, V. Bhatt, G. Saste, S. Pawar, L. Hingorani, M. Shah
A validated UHPLC-PDA with an ESI-MS/MS method has been developed for simultaneous estimation of six bioactive alkaloids (magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine) in the different extracts of the roots of Berberis aristata DC (Family:Berberdiaceae). It is an important medicinal herb native to Northern Himalaya and commonly known as ‘daruharidra’, ‘daruhaldi’, ‘Indian barberry’ or ‘tree turmeric’. An insight into the research literature uncovered reports on isoquinoline alkaloids like magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine, and berberine as major bioactives in B. aristata roots, possessing different pharmacological and therapeutic effects. In the present study, these aforementioned alkaloids were separated on Phenomenex Luna®, 5 µm-C8 analytical column. The HPLC-MS analysis was performed at a flow rate of 0.90 mL min−1. Each alkaloid that is resolved was characterized by precursor ions and fragment ions with electrospray ionization (ESI) source in both positive and negative ionization using scan mode. The limit of detections (LODs) were 0.087, 0.727, 0.035, 0.124, 0.782 and 0.794 μg mL−1 for magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine, respectively. The proposed UHPLC-PDA method was fully validated according to international (ICH) guidelines and was found to be selective, sensitive and highly accurate for the concomitant estimation of the aforementioned symbolic bio-markers of B. aristata roots.
采用ESI-MS/MS方法对马兜铃小檗（小檗科）不同根提取物中的六种生物活性生物碱（厚朴碱、小檗胺、小柱胺、药根碱、巴马汀和黄连素）进行了同时测定。它是一种重要的草药，原产于喜马拉雅北部，通常被称为“daruharidra”、“daruhaldi”、“Indian barberry”或“tree turmeric”。深入研究文献发现，异喹啉生物碱如马格尼碱、小檗胺、小柱胺、药根碱、巴马汀和黄连素是马兜铃根中的主要生物活性物质，具有不同的药理和治疗作用。在本研究中，上述生物碱在Phenomenex Luna®5µm-C8分析柱上分离。HPLC-MS分析在0.90的流速下进行 mL min−1。使用扫描模式，用电喷雾电离（ESI）源在正电离和负电离中对解析的每种生物碱进行前体离子和碎片离子的表征。检出限分别为0.087、0.727、0.035、0.124、0.782和0.794 μg mL−1分别用于马格尼碱、小檗胺、小柱胺、药根碱、巴马汀和黄连素。根据国际（ICH）指南，所提出的UHPLC-PDA方法得到了充分验证，并被发现对上述马兜铃根的象征性生物标记物的同时估计具有选择性、敏感性和高度准确。
{"title":"Development of validated UHPLC–PDA with ESI–MS-MS method for concurrent estimation of magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine in Berberis aristata","authors":"Ishita A. Basera, A. Girme, V. Bhatt, G. Saste, S. Pawar, L. Hingorani, M. Shah","doi":"10.1556/1326.2021.00960","DOIUrl":"https://doi.org/10.1556/1326.2021.00960","url":null,"abstract":"\u0000 A validated UHPLC-PDA with an ESI-MS/MS method has been developed for simultaneous estimation of six bioactive alkaloids (magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine) in the different extracts of the roots of Berberis aristata DC (Family:Berberdiaceae). It is an important medicinal herb native to Northern Himalaya and commonly known as ‘daruharidra’, ‘daruhaldi’, ‘Indian barberry’ or ‘tree turmeric’. An insight into the research literature uncovered reports on isoquinoline alkaloids like magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine, and berberine as major bioactives in B. aristata roots, possessing different pharmacological and therapeutic effects. In the present study, these aforementioned alkaloids were separated on Phenomenex Luna®, 5 µm-C8 analytical column. The HPLC-MS analysis was performed at a flow rate of 0.90 mL min−1. Each alkaloid that is resolved was characterized by precursor ions and fragment ions with electrospray ionization (ESI) source in both positive and negative ionization using scan mode. The limit of detections (LODs) were 0.087, 0.727, 0.035, 0.124, 0.782 and 0.794 μg mL−1 for magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine, respectively. The proposed UHPLC-PDA method was fully validated according to international (ICH) guidelines and was found to be selective, sensitive and highly accurate for the concomitant estimation of the aforementioned symbolic bio-markers of B. aristata roots.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-10-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49173326","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}
The current study explores a design and development of the simple, fast, green and selective novel method of UPLC to quantify pitavastatin and ezetimibe simultaneously. The combined approach of Green Analytical Method with Quality by Design-based risk assessment was done using the Ishikawa fishbone diagram followed by a rotatable central composite design used for the optimization. The optimal chromatographic separation was attained through a mobile phase of 72: 28% v/v ethanol and 0.1% orthophosphoric acid (pH 3.5), with a 0.31 mL min−1 flow rate. The developed UPLC-PDA method was sensitive and specific for pitavastatin and ezetimibe, with linearity ranging from 2 to 30, 10–150 μg mL−1 with an R2 of 0.9999 and 0.9997, respectively. The forced degradation study of stability-indicating assay results shows the degradation in respective stress conditions. The developed UPLC method was validated and found to have sensible results with good linearity, accuracy and precision. Further, the greenness was evaluated using five states of art metrics like NEMI, GAPI, AES, AMGS, and AGREE metrics and found the greenest results. Based on the results we concluded that the developed UPLC method could be efficient for the simultaneous determination of pitavastatin and ezetimibe in bulk and tablet dosage.
{"title":"Estimation of pitavastatin and ezetimibe using UPLC by a combined approach of analytical quality by design with green analytical technique","authors":"Hemanth Kumar Chanduluru, Abimanyu Sugumaran","doi":"10.1556/1326.2021.00949","DOIUrl":"https://doi.org/10.1556/1326.2021.00949","url":null,"abstract":"\u0000 The current study explores a design and development of the simple, fast, green and selective novel method of UPLC to quantify pitavastatin and ezetimibe simultaneously. The combined approach of Green Analytical Method with Quality by Design-based risk assessment was done using the Ishikawa fishbone diagram followed by a rotatable central composite design used for the optimization. The optimal chromatographic separation was attained through a mobile phase of 72: 28% v/v ethanol and 0.1% orthophosphoric acid (pH 3.5), with a 0.31 mL min−1 flow rate. The developed UPLC-PDA method was sensitive and specific for pitavastatin and ezetimibe, with linearity ranging from 2 to 30, 10–150 μg mL−1 with an R2 of 0.9999 and 0.9997, respectively. The forced degradation study of stability-indicating assay results shows the degradation in respective stress conditions. The developed UPLC method was validated and found to have sensible results with good linearity, accuracy and precision. Further, the greenness was evaluated using five states of art metrics like NEMI, GAPI, AES, AMGS, and AGREE metrics and found the greenest results. Based on the results we concluded that the developed UPLC method could be efficient for the simultaneous determination of pitavastatin and ezetimibe in bulk and tablet dosage.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45589161","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}
Chen Chen, Jingjing Li, F. Xiong, Bo Wang, Yuanming Xiao, Guo-ying Zhou
Anisodus tanguticus (Maxim.) Pascher is an important Tibetan folk medicine and the source of tropane alkaloids (TAs) grown in Qinghai-Tibet Plateau. There are marked differences in quality of A. tanguticus from geographic areas. The aim of present research was to establish a method for the quantitative analysis of TAs coupled with chemometrics analysis to trace geographical origins. Qualitative analysis of TAs in A. tanguticus was carried out using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and quantitative analysis of TAs in different plant organs from different geographical origin was achieved. Contents of TAs were subjected to the principal component analysis, and orthogonal partial least-squares discriminant analysis. The contents of the three marker compounds (anisodamine, anisodine and atropine) in the roots and acrial parts of A. tanguticus were positive correlated and varied significantly from different geographical origins. Principal component analysis, and orthogonal partial least-squares discriminant analysis results showed excellent discrimination between different geographical origin of A. tanguticus. This study could provide comprehensive evaluation and further utilization of A. tanguticus resources.
{"title":"Multivariate statistical analysis of tropane alkaloids in Anisodus tanguticus (Maxim.) Pascher from different regions to trace geographical origins","authors":"Chen Chen, Jingjing Li, F. Xiong, Bo Wang, Yuanming Xiao, Guo-ying Zhou","doi":"10.1556/1326.2021.00952","DOIUrl":"https://doi.org/10.1556/1326.2021.00952","url":null,"abstract":"\u0000 \u0000 Anisodus tanguticus (Maxim.) Pascher is an important Tibetan folk medicine and the source of tropane alkaloids (TAs) grown in Qinghai-Tibet Plateau. There are marked differences in quality of A. tanguticus from geographic areas. The aim of present research was to establish a method for the quantitative analysis of TAs coupled with chemometrics analysis to trace geographical origins. Qualitative analysis of TAs in A. tanguticus was carried out using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry and quantitative analysis of TAs in different plant organs from different geographical origin was achieved. Contents of TAs were subjected to the principal component analysis, and orthogonal partial least-squares discriminant analysis. The contents of the three marker compounds (anisodamine, anisodine and atropine) in the roots and acrial parts of A. tanguticus were positive correlated and varied significantly from different geographical origins. Principal component analysis, and orthogonal partial least-squares discriminant analysis results showed excellent discrimination between different geographical origin of A. tanguticus. This study could provide comprehensive evaluation and further utilization of A. tanguticus resources.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-09-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49265952","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}
Joliana F Farid, N. Mostafa, Hebatallah M Essam, Y. Fayez
Due to the wide applicability of separation techniques that rely on the property of differential migration in pharmaceutical formulations analysis, different analytical strategies have been proposed to resolve mixtures of multi-components pharmaceuticals. Three separation methods were developed and validated for the simultaneous determination of Paracetamol (PAR), Pseudoephedrine HCl (PSE) and Chlorpheniramine maleate (CHP). The first method is a thin-layer chromatographic (TLC) separation, followed by densitometric measurement. The separation was carried out on aluminium sheet of silica gel 60 F254 using ethanol:chloroform:ammonia (1:7:0.4, by volume) as the mobile phase. Determination of PAR, PSE and CHP was successfully applied over the concentration ranges of 3–25 µg/band, 0.5–10 µg/band and 0.1–6 µg/band, respectively. The second method is HPLC separation that was achieved on C18 column using the mobile phase acetonitrile:phosphate buffer pH 5 (10:90, v/v) at a flow rate 1 mL min−1. PAR, PSE and CHP were determined by HPLC in concentration ranges of 5–400 μg mL−1, 2–40 μg mL−1 and 0.5–16 μg mL−1, respectively. The third method is a capillary electrophoresis (CE) separation. The electrophoretic separation was achieved using 20 mM phosphate buffer (pH 6.5) at 20 kV. The linearity was reached over concentration ranges of 30–250 μg mL−1, 5–50 μg mL−1 and 0.8–20 μg mL−1 for PAR, PSE and CHP, respectively. The developed methods were validated with respect to linearity, precision, accuracy and system suitability. The proposed methods were successfully applied for bulk powder and dosage form analysis with RSD of precision <2%. Moreover, statistical comparison with the official methods confirms the methods' validity.
{"title":"Implementation of different separation techniques for resolving ternary mixture of Paracetamol, Pseudoephedrine Hydrochloride and Chlorpheniramine maleate with further quantification","authors":"Joliana F Farid, N. Mostafa, Hebatallah M Essam, Y. Fayez","doi":"10.1556/1326.2021.00954","DOIUrl":"https://doi.org/10.1556/1326.2021.00954","url":null,"abstract":"\u0000 Due to the wide applicability of separation techniques that rely on the property of differential migration in pharmaceutical formulations analysis, different analytical strategies have been proposed to resolve mixtures of multi-components pharmaceuticals. Three separation methods were developed and validated for the simultaneous determination of Paracetamol (PAR), Pseudoephedrine HCl (PSE) and Chlorpheniramine maleate (CHP). The first method is a thin-layer chromatographic (TLC) separation, followed by densitometric measurement. The separation was carried out on aluminium sheet of silica gel 60 F254 using ethanol:chloroform:ammonia (1:7:0.4, by volume) as the mobile phase. Determination of PAR, PSE and CHP was successfully applied over the concentration ranges of 3–25 µg/band, 0.5–10 µg/band and 0.1–6 µg/band, respectively. The second method is HPLC separation that was achieved on C18 column using the mobile phase acetonitrile:phosphate buffer pH 5 (10:90, v/v) at a flow rate 1 mL min−1. PAR, PSE and CHP were determined by HPLC in concentration ranges of 5–400 μg mL−1, 2–40 μg mL−1 and 0.5–16 μg mL−1, respectively. The third method is a capillary electrophoresis (CE) separation. The electrophoretic separation was achieved using 20 mM phosphate buffer (pH 6.5) at 20 kV. The linearity was reached over concentration ranges of 30–250 μg mL−1, 5–50 μg mL−1 and 0.8–20 μg mL−1 for PAR, PSE and CHP, respectively. The developed methods were validated with respect to linearity, precision, accuracy and system suitability. The proposed methods were successfully applied for bulk powder and dosage form analysis with RSD of precision <2%. Moreover, statistical comparison with the official methods confirms the methods' validity.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47230264","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}
M. A. El-Shazly, Ahmed A. Hamed, H. Kabary, M. Ghareeb
The therapeutical applications of ornamental plants have been categorized to be of a great effectiveness in multiple industries from ancient times until present days. Pluchea dioscoridis is widely known Egyptian wooden plant that has been extensively applied for different medicinal purposes. In this study, LC-ESI-MS/MS analysis of the potent antimicrobial ethyl acetate and n-butanol extracts of P. dioscoridis leaves led to identification of 28 and 21 compounds, respectively. The identified compounds were categorized as phenolic acids, phenolic acids derivatives, organic acids, flavonoids (aglycones and glycosides), secoiridoids, coumarin derivatives, and gallotannins derivatives. Among them, caffeic acid 3-sulfate was the most predominate in the investigated extracts followed by ferulic acid and dicaffeoyl-quinic acid. Also, the antimicrobial potentiality of different extracts was evaluated against different pathogenic microbes including Enterobacter cloacae, Micrococcus leutus, Aeromonas hydrophila, Bacillus subtilis, Bacillus cereus, Bacillus lichneformis and Clostridium species. Furthermore, different concentrations of the most potent extract were assayed for antibacterial efficacy on growth curve kinetics against the susceptible bacteria along 4days incubation period. Our gathered data confirmed that, the antimicrobial activity against tested bacteria was different according to the solvent used in the extraction process. Mostly, all the extracts showed a wide spectrum antibacterial activity except the plant water extract which shows a mild activity against Clostridium sp. only. Based on the highest inhibition zone diameter, the ethyl acetate extract followed by butanol extract exhibited the highest inhibition zone with Micrococcus luteus and B. subtilis (20.0 and 18.5 mm) respectively. Determining the effect of ethyl acetate extract at different concentration (0, 0.66, 1.66, 3.33, 6.67, 13.34 and 20.01 mg mL−1) on M. luteus growth kinetics, the data assured that the antibacterial activity shows concentration dependent manner with the highest antibacterial activity at 20.01 mg mL−1 culture. The data also confirmed that, none of the selected concentration showed bactericidal activity in the prepared cultures, and with the prolonged incubation period the bacteria acquire resistance against the extract beginning from second or third day of incubation.
{"title":"LC-MS/MS profiling, antibiofilm, antimicrobial and bacterial growth kinetic studies of Pluchea dioscoridis extracts","authors":"M. A. El-Shazly, Ahmed A. Hamed, H. Kabary, M. Ghareeb","doi":"10.1556/1326.2021.00956","DOIUrl":"https://doi.org/10.1556/1326.2021.00956","url":null,"abstract":"\u0000 The therapeutical applications of ornamental plants have been categorized to be of a great effectiveness in multiple industries from ancient times until present days. Pluchea dioscoridis is widely known Egyptian wooden plant that has been extensively applied for different medicinal purposes. In this study, LC-ESI-MS/MS analysis of the potent antimicrobial ethyl acetate and n-butanol extracts of P. dioscoridis leaves led to identification of 28 and 21 compounds, respectively. The identified compounds were categorized as phenolic acids, phenolic acids derivatives, organic acids, flavonoids (aglycones and glycosides), secoiridoids, coumarin derivatives, and gallotannins derivatives. Among them, caffeic acid 3-sulfate was the most predominate in the investigated extracts followed by ferulic acid and dicaffeoyl-quinic acid. Also, the antimicrobial potentiality of different extracts was evaluated against different pathogenic microbes including Enterobacter cloacae, Micrococcus leutus, Aeromonas hydrophila, Bacillus subtilis, Bacillus cereus, Bacillus lichneformis and Clostridium species. Furthermore, different concentrations of the most potent extract were assayed for antibacterial efficacy on growth curve kinetics against the susceptible bacteria along 4days incubation period. Our gathered data confirmed that, the antimicrobial activity against tested bacteria was different according to the solvent used in the extraction process. Mostly, all the extracts showed a wide spectrum antibacterial activity except the plant water extract which shows a mild activity against Clostridium sp. only. Based on the highest inhibition zone diameter, the ethyl acetate extract followed by butanol extract exhibited the highest inhibition zone with Micrococcus luteus and B. subtilis (20.0 and 18.5 mm) respectively. Determining the effect of ethyl acetate extract at different concentration (0, 0.66, 1.66, 3.33, 6.67, 13.34 and 20.01 mg mL−1) on M. luteus growth kinetics, the data assured that the antibacterial activity shows concentration dependent manner with the highest antibacterial activity at 20.01 mg mL−1 culture. The data also confirmed that, none of the selected concentration showed bactericidal activity in the prepared cultures, and with the prolonged incubation period the bacteria acquire resistance against the extract beginning from second or third day of incubation.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48737931","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}
A sweeping micellar electrokinetic chromatography (sweeping-MEKC) method was developed for the determination of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol in cosmetics. Several parameters affecting sweeping-MEKC method were studied systematically and the separation conditions were optimized as 20 mM NaH2PO4–110 mM SDS and 40% (v/v) MeOH (pH 2.4), with −22 kV applied voltage and UV detection at 230 nm. The sample matrix is 60 mmol L−1 NaH2PO4 and sample introduction was performed at 3 psi for 6 s. Separation of the four naphthalenediols was completed in less than 17 min. Limit of detection (LOD) and limit of quantitation (LOQ) are 0.0045∼0.0094 μg mL−1 and 0.015∼0.031 μg mL−1. Linear relationship (r 2 > 0.999) is satisfactory at the range of 0.1–10 μg mL−1. The developed method has been successfully applied to the determination of the four naphthalenediols in real cosmetic samples, with recoveries in foundation, sun cream and lotion in the range of 92.3%∼106.8% and relative standard deviation (RSD) less than 4.15%. A HPLC method described in the National Standards of the People’s Republic of China was carried out for the comparison with the proposed method. The results showed that the proposed sweeping-MEKC method has the advantages of fast, low cost with comparative sensitivity.
建立了化妆品中1,7-萘二醇、2,3-萘二醇、1,5-萘二醇和2,7-萘二醇的扫胶束电动色谱法。系统研究了影响扫频MEKC法的几个参数，并将分离条件优化为20 mM NaH2PO4–110 mM SDS和40%（v/v）MeOH（pH 2.4），施加−22 kV电压，在230下进行紫外线检测 nm。样本矩阵为60 mmol L−1 NaH2PO4，样品引入在3 psi下进行6 s.四种萘二醇的分离在不到17分钟的时间内完成 最小检测限（LOD）和定量限（LOQ）为0.0045～0.0094 μg mL−1和0.015～0.031 μg mL−1。线性关系（r2>0.999）在0.1–10范围内是令人满意的 μg mL−1。该方法已成功应用于化妆品样品中四种萘二醇的测定，防晒霜和乳液的含量在92.3%～106.8%之间，相对标准偏差（RSD）小于4.15%。结果表明，所提出的扫频MEKC方法具有快速、低成本和相对灵敏度的优点。
{"title":"Determination of four naphthalenediols in cosmetic samples by sweeping-micellar electrokinetic chromatography and a comparison with HPLC","authors":"Qian Wang, Xiaobin Li, Zhihan Zheng, Huitao Liu, Yuan Gao","doi":"10.1556/1326.2021.00942","DOIUrl":"https://doi.org/10.1556/1326.2021.00942","url":null,"abstract":"\u0000 A sweeping micellar electrokinetic chromatography (sweeping-MEKC) method was developed for the determination of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol in cosmetics. Several parameters affecting sweeping-MEKC method were studied systematically and the separation conditions were optimized as 20 mM NaH2PO4–110 mM SDS and 40% (v/v) MeOH (pH 2.4), with −22 kV applied voltage and UV detection at 230 nm. The sample matrix is 60 mmol L−1 NaH2PO4 and sample introduction was performed at 3 psi for 6 s. Separation of the four naphthalenediols was completed in less than 17 min. Limit of detection (LOD) and limit of quantitation (LOQ) are 0.0045∼0.0094 μg mL−1 and 0.015∼0.031 μg mL−1. Linear relationship (r\u0000 2 > 0.999) is satisfactory at the range of 0.1–10 μg mL−1. The developed method has been successfully applied to the determination of the four naphthalenediols in real cosmetic samples, with recoveries in foundation, sun cream and lotion in the range of 92.3%∼106.8% and relative standard deviation (RSD) less than 4.15%. A HPLC method described in the National Standards of the People’s Republic of China was carried out for the comparison with the proposed method. The results showed that the proposed sweeping-MEKC method has the advantages of fast, low cost with comparative sensitivity.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46152660","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}
Two sensitive and effective methods were developed for the detection of catecholamines and related biogenic amines (dopamine, epinephrine, norepinephrine, serotonin, levodopa and tyramine) using high performance liquid chromatography with fluorescence detection and capillary electrophoresis with laser-induced fluorescence detection. A BODIPY fluorescent dye, 1, 3, 5, 7-tetramethyl-8-(N-hydroxysuccinimidyl propionic ester)-difluoroboradiaza- s-indacene was used as pre-column derivatization reagent. The separation and derivatization conditions were optimized in detail. In high performance liquid chromatography with fluorescence detection method, the derivatization reaction was completed at 35 °C for 20 min. At the wavelength of λex/λem = 493 nm/513 nm, dopamine, epinephrine, norepinephrine, and levodopa derivatives achieved baseline separation within 15 min. The limits of detection (S/N = 3) were 1.0, 2.0, 5.0, and 0.5 nmol/L, respectively. In capillary electrophoresis with laser-induced fluorescence detection method, the derivatization reaction was completed at 25 °C for 20 min. Serotonin, tyramine and dopamine derivatives reached baseline separation within 10 min at the wavelength of λex = 473 nm. The limits of detection (S/N = 3) for serotonin, tyramine, and dopamine were 0.3, 0.02, and 0.2 nmol/L, respectively. The amino compounds in human serum and urine samples were detected successfully, and the recoveries were 93.3%–106.7% and 91.0%–103.1%, respectively.
{"title":"Analysis of neurotransmitter catecholamines and related amines in human urine and serum by chromatography and capillary electrophoresis with 1, 3, 5, 7-tetramethyl-8-(N-hydroxysuccinimidyl propionic ester)-difluoro-boradiaza-s-indacene","authors":"Liwei Cao, Lizhen Wu, Hailan Zhong, Hao Wu, Siyu Zhang, Jianxin Meng, Fengyu Li","doi":"10.1556/1326.2021.00924","DOIUrl":"https://doi.org/10.1556/1326.2021.00924","url":null,"abstract":"Two sensitive and effective methods were developed for the detection of catecholamines and related biogenic amines (dopamine, epinephrine, norepinephrine, serotonin, levodopa and tyramine) using high performance liquid chromatography with fluorescence detection and capillary electrophoresis with laser-induced fluorescence detection. A BODIPY fluorescent dye, 1, 3, 5, 7-tetramethyl-8-(N-hydroxysuccinimidyl propionic ester)-difluoroboradiaza- s-indacene was used as pre-column derivatization reagent. The separation and derivatization conditions were optimized in detail. In high performance liquid chromatography with fluorescence detection method, the derivatization reaction was completed at 35 °C for 20 min. At the wavelength of λex/λem = 493 nm/513 nm, dopamine, epinephrine, norepinephrine, and levodopa derivatives achieved baseline separation within 15 min. The limits of detection (S/N = 3) were 1.0, 2.0, 5.0, and 0.5 nmol/L, respectively. In capillary electrophoresis with laser-induced fluorescence detection method, the derivatization reaction was completed at 25 °C for 20 min. Serotonin, tyramine and dopamine derivatives reached baseline separation within 10 min at the wavelength of λex = 473 nm. The limits of detection (S/N = 3) for serotonin, tyramine, and dopamine were 0.3, 0.02, and 0.2 nmol/L, respectively. The amino compounds in human serum and urine samples were detected successfully, and the recoveries were 93.3%–106.7% and 91.0%–103.1%, respectively.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43197397","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}
Maharshi Thalla, Aishwarya Jala, Roshan M. Borkar, Subhamoy Banerjee
Pyrazinamide (PZA), a medication for tuberculosis, has high aqueous solubility and low permeability, undergoes extensive liver metabolism, and exhibits liver toxicity through its metabolites. To avoid this, PZA in lipid core-shell nanoarchitectonics has been formulated to target lymphatic uptake and provide metabolic stability to the incorporated drug. The UPLC-MS/MS method for reliable in vitro quantitative analysis of pyrazinamide (PZA) in lipid core-shell nanoarchitectonics as per ICH guidance was developed and validated using the HILIC column. The developed UPLC-MS/MS method is a simple, precise, accurate, reproducible, and sensitive method for the estimation of PZA in PZA-loaded lipid core-shell nanoarchitectonics for the in vitro determination of % entrapment efficiency, % loading of pyrazinamide, and microsomal stability of lipid core-shell nanoarchitectonics in human liver microsomes. The % entrapment efficiency was found to be 42.72% (±12.60). Lipid nanoarchitectonics was found to be stable in human liver microsomes, where %QH was found to be 6.20%, that is, low clearance. Thus, this formulation is suitable for preventing PZA-mediated extensive liver metabolism. These findings are relevant for the development of other lipid-mediated, suitable, stable nanoformulations containing PZA through various in vitro methods.
{"title":"Development and validation of UPLC-MS/MS method for in vitro quantitative analysis of pyrazinamide in lipid core-shell nanoarchitectonics for improved metabolic stability","authors":"Maharshi Thalla, Aishwarya Jala, Roshan M. Borkar, Subhamoy Banerjee","doi":"10.1556/1326.2021.00916","DOIUrl":"https://doi.org/10.1556/1326.2021.00916","url":null,"abstract":"Pyrazinamide (PZA), a medication for tuberculosis, has high aqueous solubility and low permeability, undergoes extensive liver metabolism, and exhibits liver toxicity through its metabolites. To avoid this, PZA in lipid core-shell nanoarchitectonics has been formulated to target lymphatic uptake and provide metabolic stability to the incorporated drug. The UPLC-MS/MS method for reliable in vitro quantitative analysis of pyrazinamide (PZA) in lipid core-shell nanoarchitectonics as per ICH guidance was developed and validated using the HILIC column. The developed UPLC-MS/MS method is a simple, precise, accurate, reproducible, and sensitive method for the estimation of PZA in PZA-loaded lipid core-shell nanoarchitectonics for the in vitro determination of % entrapment efficiency, % loading of pyrazinamide, and microsomal stability of lipid core-shell nanoarchitectonics in human liver microsomes. The % entrapment efficiency was found to be 42.72% (±12.60). Lipid nanoarchitectonics was found to be stable in human liver microsomes, where %QH was found to be 6.20%, that is, low clearance. Thus, this formulation is suitable for preventing PZA-mediated extensive liver metabolism. These findings are relevant for the development of other lipid-mediated, suitable, stable nanoformulations containing PZA through various in vitro methods.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46713931","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}
Yahua Yang, Zhizhong Xue, Ran Meng, Zhentao Wu, Zhaojia Li, Wei Zhang, Shihui Ge
A sensitive and rapid method using HPLC-MS/MS was developed for the determination of eight glucocorticoids residues in chicken muscle simultaneously by Turbo Flow. The eight glucocorticoids were prednisone, prednisolone, hydrocortisone, methylprednisolone, dexamethasone, betamethasone, beclomethasone and fludrocortisones. Samples were extracted with ethyl acetate and on-line cleaned up through a Turbo Flow solid-phase extraction column without time-consuming pretreatment before HPLC-MS/MS analysis. Sample pretreatment conditions, Turbo Flow conditions and mass spectral parameters were optimized and obtained eight glucocorticoids calibration curves. These curves showed good linearity over the concentration from 0.2 μg/kg to 50 μg/kg with an average recovery from 71.63% to 117.36%. This method could be applied on real samples and provided simple, rapid, sensitive and highly selective analysis, which made it feasible to be adopted in food inspection organizations or carry out quantitative analysis for other banned substance.
{"title":"Determination of eight kinds of glucocorticoids residues in chicken muscle with on-line clean up combined HPLC-MS/MS","authors":"Yahua Yang, Zhizhong Xue, Ran Meng, Zhentao Wu, Zhaojia Li, Wei Zhang, Shihui Ge","doi":"10.1556/1326.2021.00933","DOIUrl":"https://doi.org/10.1556/1326.2021.00933","url":null,"abstract":"A sensitive and rapid method using HPLC-MS/MS was developed for the determination of eight glucocorticoids residues in chicken muscle simultaneously by Turbo Flow. The eight glucocorticoids were prednisone, prednisolone, hydrocortisone, methylprednisolone, dexamethasone, betamethasone, beclomethasone and fludrocortisones. Samples were extracted with ethyl acetate and on-line cleaned up through a Turbo Flow solid-phase extraction column without time-consuming pretreatment before HPLC-MS/MS analysis. Sample pretreatment conditions, Turbo Flow conditions and mass spectral parameters were optimized and obtained eight glucocorticoids calibration curves. These curves showed good linearity over the concentration from 0.2 μg/kg to 50 μg/kg with an average recovery from 71.63% to 117.36%. This method could be applied on real samples and provided simple, rapid, sensitive and highly selective analysis, which made it feasible to be adopted in food inspection organizations or carry out quantitative analysis for other banned substance.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43785590","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}
The quality of pesticide formulations has an impact on the crop safety, environment and human health. Therefore, the development of new analytical methods for the determination of active substances in pesticide formulations in order to control their quality, as well as, their residues in food samples in order to ensure food safety, is always welcome. A new, simple, precise and accurate normal-phase high-performance liquid chromatography (NP-HPLC) method for determination of an active ingredient malathion in the commercial emulsifiable concentrate pesticide product has been developed and validated. The analysis was carried out on a LiChrosorb CN (250 x 4 mm, 5 μm) analytical column using isocratic elution with mobile phase consisted of n-hexane and dichloromethane (80/20, v/v), flow rate of 1 mL/min, constant column temperature at 25 °C and ultraviolet diode-array detection at 220 nm. The obtained values for multiple correlation coefficients (R2 ≥ 0.9990), relative standard deviation of retention times, peak areas and heights (RSD ≤ 1.14%), recoveries ranged from 98.97 to 101.62%, revealed that the developed method has a satisfactory linearity, precision and accuracy. Also, the developed method was successfully applied for determination of malathion residues in apple juice samples, after preliminary sample preparation using solid-phase extraction. Specificity, selectivity, linearity, matrix effect, precision and accuracy were tested in order to validation of this method. The obtained results were in acceptable ranges and indicated that the developed method is suitable for routine determination of malathion in the pesticide formulation, as well as for determination of malathion residues in apple juice samples. The run time of HPLC analysis was about 6 min.
农药制剂的质量影响着作物安全、环境和人类健康。因此，开发新的分析方法来测定农药制剂中的活性物质，以控制其质量，以及控制其在食品样品中的残留，以确保食品安全，始终是受欢迎的。建立了一种新的、简便、精密、准确的正相高效液相色谱法（NP-HPLC）测定市售乳油农药产品中活性成分马拉硫磷的方法，并进行了验证。分析是在LiChrosorb CN（250 x 4 毫米，5 μm）分析柱，流动相为正己烷和二氯甲烷（80/20，v/v），流速为1 mL/min，柱温恒定在25 220°C和紫外线二极管阵列检测 nm。多元相关系数R2≥0.9990，保留时间、峰面积和峰高的相对标准偏差（RSD≤1.14%），回收率范围为98.97～101.62%，表明该方法具有良好的线性、精密度和准确度。采用固相萃取法对苹果汁样品进行了初步制备，并成功地应用于苹果汁样品中马拉硫磷残留量的测定。对该方法的特异性、选择性、线性、基质效应、精密度和准确度进行了测试，以验证该方法的有效性。结果在可接受的范围内，表明该方法适用于农药制剂中马拉硫磷的常规测定，也适用于苹果汁样品中马拉硫磷残留量的测定。HPLC分析的运行时间约为6 最小。
{"title":"Determination of malathion and its residues by normal-phase high-performance liquid chromatography method","authors":"L. Velkoska-Markovska, B. Petanovska-Ilievska","doi":"10.1556/1326.2021.00935","DOIUrl":"https://doi.org/10.1556/1326.2021.00935","url":null,"abstract":"The quality of pesticide formulations has an impact on the crop safety, environment and human health. Therefore, the development of new analytical methods for the determination of active substances in pesticide formulations in order to control their quality, as well as, their residues in food samples in order to ensure food safety, is always welcome. A new, simple, precise and accurate normal-phase high-performance liquid chromatography (NP-HPLC) method for determination of an active ingredient malathion in the commercial emulsifiable concentrate pesticide product has been developed and validated. The analysis was carried out on a LiChrosorb CN (250 x 4 mm, 5 μm) analytical column using isocratic elution with mobile phase consisted of n-hexane and dichloromethane (80/20, v/v), flow rate of 1 mL/min, constant column temperature at 25 °C and ultraviolet diode-array detection at 220 nm. The obtained values for multiple correlation coefficients (R2 ≥ 0.9990), relative standard deviation of retention times, peak areas and heights (RSD ≤ 1.14%), recoveries ranged from 98.97 to 101.62%, revealed that the developed method has a satisfactory linearity, precision and accuracy. Also, the developed method was successfully applied for determination of malathion residues in apple juice samples, after preliminary sample preparation using solid-phase extraction. Specificity, selectivity, linearity, matrix effect, precision and accuracy were tested in order to validation of this method. The obtained results were in acceptable ranges and indicated that the developed method is suitable for routine determination of malathion in the pesticide formulation, as well as for determination of malathion residues in apple juice samples. The run time of HPLC analysis was about 6 min.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43055619","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}
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