首页 > 最新文献

Analytical Chemistry Insights最新文献

英文 中文
Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges. 醋酸甲羟孕酮阴道内海绵的高效液相色谱分析方法验证及稳定性研究。
Pub Date : 2017-02-20 eCollection Date: 2017-01-01 DOI: 10.1177/1177390117690152
Nidal Batrawi, Shorouq Wahdan, Murad Abualhasan

Medroxyprogesterone acetate is widely used in veterinary medicine as intravaginal dosage for the synchronization of breeding cycle in ewes and goats. The main goal of this study was to develop reverse-phase high-performance liquid chromatography method for the quantification of medroxyprogesterone acetate in veterinary vaginal sponges. A single high-performance liquid chromatography/UV isocratic run was used for the analytical assay of the active ingredient medroxyprogesterone. The chromatographic system consisted of a reverse-phase C18 column as the stationary phase and a mixture of 60% acetonitrile and 40% potassium dihydrogen phosphate buffer as the mobile phase; the pH was adjusted to 5.6. The method was validated according to the International Council for Harmonisation (ICH) guidelines. Forced degradation studies were also performed to evaluate the stability-indicating properties and specificity of the method. Medroxyprogesterone was eluted at 5.9 minutes. The linearity of the method was confirmed in the range of 0.0576 to 0.1134 mg/mL (R2 > 0.999). The limit of quantification was shown to be 3.9 µg/mL. Precision and accuracy ranges were found to be %RSD <0.2 and 98% to 102%, respectively. Medroxyprogesterone capacity factor value of 2.1, tailing factor value of 1.03, and resolution value of 3.9 were obtained in accordance with ICH guidelines. Based on the obtained results, a rapid, precise, accurate, sensitive, and cost-effective analysis procedure was proposed for quantitative determination of medroxyprogesterone in vaginal sponges. This analytical method is the only available method to analyse medroxyprogesterone in veterinary intravaginal dosage form.

醋酸甲孕酮在兽医学中广泛应用于母羊和山羊的阴道内剂量同步繁殖周期。本研究的主要目的是建立反相高效液相色谱法定量兽用阴道海绵中醋酸甲孕酮的方法。采用高效液相色谱/紫外分光光度法对甲羟孕酮进行分析。色谱系统以反相C18柱为固定相,60%乙腈和40%磷酸二氢钾缓冲液的混合物为流动相;pH值调整为5.6。该方法根据国际协调理事会(ICH)指南进行了验证。还进行了强制降解研究,以评估该方法的稳定性和特异性。甲孕酮在5.9分钟洗脱。在0.0576 ~ 0.1134 mg/mL范围内线性良好(R2 > 0.999)。定量限为3.9µg/mL。精密度和准确度范围为%RSD
{"title":"Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges.","authors":"Nidal Batrawi,&nbsp;Shorouq Wahdan,&nbsp;Murad Abualhasan","doi":"10.1177/1177390117690152","DOIUrl":"https://doi.org/10.1177/1177390117690152","url":null,"abstract":"<p><p>Medroxyprogesterone acetate is widely used in veterinary medicine as intravaginal dosage for the synchronization of breeding cycle in ewes and goats. The main goal of this study was to develop reverse-phase high-performance liquid chromatography method for the quantification of medroxyprogesterone acetate in veterinary vaginal sponges. A single high-performance liquid chromatography/UV isocratic run was used for the analytical assay of the active ingredient medroxyprogesterone. The chromatographic system consisted of a reverse-phase C18 column as the stationary phase and a mixture of 60% acetonitrile and 40% potassium dihydrogen phosphate buffer as the mobile phase; the pH was adjusted to 5.6. The method was validated according to the International Council for Harmonisation (ICH) guidelines. Forced degradation studies were also performed to evaluate the stability-indicating properties and specificity of the method. Medroxyprogesterone was eluted at 5.9 minutes. The linearity of the method was confirmed in the range of 0.0576 to 0.1134 mg/mL (<i>R</i><sup>2</sup> > 0.999). The limit of quantification was shown to be 3.9 µg/mL. Precision and accuracy ranges were found to be %RSD <0.2 and 98% to 102%, respectively. Medroxyprogesterone capacity factor value of 2.1, tailing factor value of 1.03, and resolution value of 3.9 were obtained in accordance with ICH guidelines. Based on the obtained results, a rapid, precise, accurate, sensitive, and cost-effective analysis procedure was proposed for quantitative determination of medroxyprogesterone in vaginal sponges. This analytical method is the only available method to analyse medroxyprogesterone in veterinary intravaginal dosage form.</p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2017-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1177/1177390117690152","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34966271","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 5
Insight into Biochemical Characterization of Plant Sesquiterpene Synthases 植物倍半萜合成酶的生化特性研究
Pub Date : 2016-09-29 DOI: 10.4137/ACI.S40292
Tom Manczak, H. T. Simonsen
A fast and reproducible protocol was established for enzymatic characterization of plant sesquiterpene synthases that can incorporate radioactivity in their products. The method utilizes the 96-well format in conjunction with cluster tubes and enables processing of >200 samples a day. Along with reduced reagent usage, it allows further reduction in the use of radioactive isotopes and flammable organic solvents. The sesquiterpene synthases previously characterized were expressed in yeast, and the plant-derived Thapsia garganica kunzeaol synthase TgTPS2 was tested in this method. KM for TgTPS2 was found to be 0.55 μM; the turnover number, kcat, was found to be 0.29 s−1, kcat for TgTPS2 is in agreement with that of terpene synthases of other plants, and kcat/KM was found to be 0.53 s−1 μM−1 for TgTPS2. The kinetic parameters were in agreement with previously published data.
建立了一种快速、可重复的植物倍半萜合成酶的酶学表征方法,该方法可以将放射性纳入其产物中。该方法将96孔格式与簇管结合使用,每天可处理100 ~ 200个样品。随着试剂使用量的减少,它可以进一步减少放射性同位素和易燃有机溶剂的使用。先前鉴定的倍半萜合成酶在酵母中表达,本方法检测了植物源性甘菊合成酶TgTPS2。TgTPS2的KM为0.55 μM;TgTPS2的周转数kcat为0.29 s−1,与其他植物萜类合成酶的kcat一致,kcat/KM为0.53 s−1 μM−1。动力学参数与先前发表的数据一致。
{"title":"Insight into Biochemical Characterization of Plant Sesquiterpene Synthases","authors":"Tom Manczak, H. T. Simonsen","doi":"10.4137/ACI.S40292","DOIUrl":"https://doi.org/10.4137/ACI.S40292","url":null,"abstract":"A fast and reproducible protocol was established for enzymatic characterization of plant sesquiterpene synthases that can incorporate radioactivity in their products. The method utilizes the 96-well format in conjunction with cluster tubes and enables processing of >200 samples a day. Along with reduced reagent usage, it allows further reduction in the use of radioactive isotopes and flammable organic solvents. The sesquiterpene synthases previously characterized were expressed in yeast, and the plant-derived Thapsia garganica kunzeaol synthase TgTPS2 was tested in this method. KM for TgTPS2 was found to be 0.55 μM; the turnover number, kcat, was found to be 0.29 s−1, kcat for TgTPS2 is in agreement with that of terpene synthases of other plants, and kcat/KM was found to be 0.53 s−1 μM−1 for TgTPS2. The kinetic parameters were in agreement with previously published data.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81794701","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 of Hollow-Fiber Liquid-Phase Microextraction Method for Determination of Urinary trans,trans-Muconic Acid as a Biomarker of Benzene Exposure 中空纤维液相微萃取法测定尿中苯暴露生物标志物反式、反式粘膜酸的建立
Pub Date : 2016-09-11 DOI: 10.4137/ACI.S40177
F. Ghamari, A. Bahrami, Y. Yamini, F. G. Shahna, A. Moghimbeigi
For the first time, hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography–ultraviolet was used to extract trans,trans-muconic acid, in urine samples of workers who had been exposed to benzene. The parameters affecting the metabolite extraction were optimized as follows: the volume of sample solution was 11 mL with pH 2, liquid membrane containing dihexyl ether as the supporter, 15% (w/v) of trioctylphosphine oxide as the carrier, the time of extraction was 120 minutes, and stirring rate was 500 rpm. Organic phase impregnated in the pores of a hollow fiber was extracted into 24 µL solution of 0.05 mol L−1 Na2CO3 located inside the lumen of the fiber. Under optimized conditions, a high enrichment factor of 153–182 folds, relative recovery of 83%–92%, and detection limit of 0.001 µg mL−1 were obtained. The method was successfully applied to the analysis of ttMA in real urine samples.
首次采用中空纤维液相微萃取联合高效液相色谱-紫外萃取法提取苯接触工人尿液中的反式粘膜酸。对影响代谢物提取的参数进行优化:样品溶液体积为11 mL, pH为2,含二己基醚的液膜为载体,氧化三辛基膦为载体,提取时间为120 min,搅拌速度为500 rpm。将浸没在中空纤维孔隙中的有机相提取到位于纤维管腔内的24µL 0.05 mol L−1 Na2CO3溶液中。在优化条件下,获得了高富集系数为153 ~ 182倍,相对回收率为83% ~ 92%,检出限为0.001µg mL−1。该方法已成功应用于实际尿样中ttMA的分析。
{"title":"Development of Hollow-Fiber Liquid-Phase Microextraction Method for Determination of Urinary trans,trans-Muconic Acid as a Biomarker of Benzene Exposure","authors":"F. Ghamari, A. Bahrami, Y. Yamini, F. G. Shahna, A. Moghimbeigi","doi":"10.4137/ACI.S40177","DOIUrl":"https://doi.org/10.4137/ACI.S40177","url":null,"abstract":"For the first time, hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography–ultraviolet was used to extract trans,trans-muconic acid, in urine samples of workers who had been exposed to benzene. The parameters affecting the metabolite extraction were optimized as follows: the volume of sample solution was 11 mL with pH 2, liquid membrane containing dihexyl ether as the supporter, 15% (w/v) of trioctylphosphine oxide as the carrier, the time of extraction was 120 minutes, and stirring rate was 500 rpm. Organic phase impregnated in the pores of a hollow fiber was extracted into 24 µL solution of 0.05 mol L−1 Na2CO3 located inside the lumen of the fiber. Under optimized conditions, a high enrichment factor of 153–182 folds, relative recovery of 83%–92%, and detection limit of 0.001 µg mL−1 were obtained. The method was successfully applied to the analysis of ttMA in real urine samples.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80439299","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: 24
Stability-Indicating High-Performance Liquid Chromatography Assay for the Determination of Sulthiame in Pharmaceutical Dosage Forms 稳定性指示高效液相色谱法测定药物剂型中磺胺的含量
Pub Date : 2016-09-06 DOI: 10.4137/ACI.S38656
A. Haidar, S. Kabiche, E. Majoul, I. Balde, J. Fontan, S. Cisternino, J. Schlatter
A stability-indicating assay by reversed-phase high performance liquid chromatography method was developed and validated for the determination of sulthiame (STM). The chromatographic separation was achieved on a reversed-phase NovaPack C18 column and an isocratic mobile phase consisting of deionized water:methanol (70:30, v/v). The flow rate was 1.0 mL/min (ultraviolet detection at 210 nm). The STM was separated within 2.83 min. The linearity of the method was demonstrated in the range of 20.0–200.0 μg/mL and a coefficient of determination of r2 = 0.9999. The limits of detection and quantification were 4.2 and 9.5 μg/mL, respectively. The intraday and interday precisions were less than 1%. Accuracy of the method ranged from 98.3% to 101.7%, with a relative standard deviation of <1%. STM was degraded by accelerated breakdown in alkaline, acidic, or oxidative stress conditions. This method allows accurate and reliable determination of STM for drug stability assay in pharmaceutical studies.
建立了反相高效液相色谱法测定磺胺(STM)的稳定性测定方法,并进行了验证。色谱分离采用NovaPack C18反相色谱柱,等容流动相为去离子水:甲醇(70:30,v/v)。流速1.0 mL/min(紫外检测波长210 nm)。该方法在20.0 ~ 200.0 μg/mL范围内线性良好,决定系数r2 = 0.9999。检测限和定量限分别为4.2和9.5 μg/mL。日内和日间的精确度小于1%。方法准确度为98.3% ~ 101.7%,相对标准偏差<1%。在碱性、酸性或氧化应激条件下,STM通过加速分解被降解。该方法可以准确、可靠地测定STM,用于药学研究中的药物稳定性分析。
{"title":"Stability-Indicating High-Performance Liquid Chromatography Assay for the Determination of Sulthiame in Pharmaceutical Dosage Forms","authors":"A. Haidar, S. Kabiche, E. Majoul, I. Balde, J. Fontan, S. Cisternino, J. Schlatter","doi":"10.4137/ACI.S38656","DOIUrl":"https://doi.org/10.4137/ACI.S38656","url":null,"abstract":"A stability-indicating assay by reversed-phase high performance liquid chromatography method was developed and validated for the determination of sulthiame (STM). The chromatographic separation was achieved on a reversed-phase NovaPack C18 column and an isocratic mobile phase consisting of deionized water:methanol (70:30, v/v). The flow rate was 1.0 mL/min (ultraviolet detection at 210 nm). The STM was separated within 2.83 min. The linearity of the method was demonstrated in the range of 20.0–200.0 μg/mL and a coefficient of determination of r2 = 0.9999. The limits of detection and quantification were 4.2 and 9.5 μg/mL, respectively. The intraday and interday precisions were less than 1%. Accuracy of the method ranged from 98.3% to 101.7%, with a relative standard deviation of <1%. STM was degraded by accelerated breakdown in alkaline, acidic, or oxidative stress conditions. This method allows accurate and reliable determination of STM for drug stability assay in pharmaceutical studies.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-09-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87454391","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
Extraction of Honey Polyphenols: Method Development and Evidence of Cis Isomerization. 蜂蜜多酚的提取:方法发展及顺式异构化证据。
Pub Date : 2016-08-10 eCollection Date: 2016-01-01 DOI: 10.4137/ACI.S39739
Thibaut Istasse, Nicolas Jacquet, Thomas Berchem, Eric Haubruge, Bach Kim Nguyen, Aurore Richel

Honey polyphenols have been studied with the objective of relating honeys to their floral sources. Initially synthesized by plant, these polyphenols can be found in the plant's nectar, which are collected by bees, which convert the nectar into honey. Consequently, polyphenols constitute minor components of honey. The development of a solid-phase extraction method for honey polyphenols is presented in this study. The technique employs Amberlite XAD-2 adsorbent and was tested on monofloral honeys from six different plants: acacia, chestnut, eucalyptus, thyme, sunflower, and wild carrot. Analyses were performed using high-performance liquid chromatography coupled with UV detection and mass spectrometry. Several phenolic acids and flavonoids were identified: caffeic and p-coumaric acids, quercetin, kaempferol, naringenin, chrysin, and pinocembrin. Generally, the quantity of a given polyphenol in the honey was around 0.2 mg/100 g of honey, except for chestnut honey, which contained around 3.0 mg of p-coumaric acid/100 g of honey. Analyses highlighted significant formation of cis isomers for phenolic acids during the extraction despite protection from light.

研究蜂蜜多酚的目的是将蜂蜜与它们的花源联系起来。这些多酚最初是由植物合成的,可以在植物的花蜜中找到,这些花蜜是由蜜蜂收集的,蜜蜂将花蜜转化为蜂蜜。因此,多酚是蜂蜜的次要成分。研究了蜂蜜中多酚的固相萃取方法。该技术采用Amberlite XAD-2吸附剂,并对来自六种不同植物的单花蜂蜜进行了测试:金合欢、栗子、桉树、百里香、向日葵和野生胡萝卜。采用高效液相色谱法结合紫外检测和质谱法进行分析。鉴定出几种酚酸和类黄酮:咖啡酸和对香豆酸、槲皮素、山奈酚、柚皮素、菊花素和松皮素。一般来说,蜂蜜中给定多酚的含量约为0.2毫克/100克蜂蜜,除了栗子蜂蜜,它含有约3.0毫克/100克蜂蜜对香豆酸。分析强调了在提取过程中酚酸的顺式异构体的显著形成,尽管有光保护。
{"title":"Extraction of Honey Polyphenols: Method Development and Evidence of Cis Isomerization.","authors":"Thibaut Istasse,&nbsp;Nicolas Jacquet,&nbsp;Thomas Berchem,&nbsp;Eric Haubruge,&nbsp;Bach Kim Nguyen,&nbsp;Aurore Richel","doi":"10.4137/ACI.S39739","DOIUrl":"https://doi.org/10.4137/ACI.S39739","url":null,"abstract":"<p><p>Honey polyphenols have been studied with the objective of relating honeys to their floral sources. Initially synthesized by plant, these polyphenols can be found in the plant's nectar, which are collected by bees, which convert the nectar into honey. Consequently, polyphenols constitute minor components of honey. The development of a solid-phase extraction method for honey polyphenols is presented in this study. The technique employs Amberlite XAD-2 adsorbent and was tested on monofloral honeys from six different plants: acacia, chestnut, eucalyptus, thyme, sunflower, and wild carrot. Analyses were performed using high-performance liquid chromatography coupled with UV detection and mass spectrometry. Several phenolic acids and flavonoids were identified: caffeic and p-coumaric acids, quercetin, kaempferol, naringenin, chrysin, and pinocembrin. Generally, the quantity of a given polyphenol in the honey was around 0.2 mg/100 g of honey, except for chestnut honey, which contained around 3.0 mg of p-coumaric acid/100 g of honey. Analyses highlighted significant formation of cis isomers for phenolic acids during the extraction despite protection from light. </p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4137/ACI.S39739","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34324497","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 33
On the Conflicting Estimations of Pigment Site Energies in Photosynthetic Complexes: A Case Study of the CP47 Complex. 光合配合物中色素位能的冲突估计:以CP47配合物为例。
Pub Date : 2016-06-02 eCollection Date: 2016-01-01 DOI: 10.4137/ACI.S32151
Tonu Reinot, Jinhai Chen, Adam Kell, Mahboobe Jassas, Kevin C Robben, Valter Zazubovich, Ryszard Jankowiak

We focus on problems with elucidation of site energies [Formula: see text] for photosynthetic complexes (PSCs) in order to raise some genuine concern regarding the conflicting estimations propagating in the literature. As an example, we provide a stern assessment of the site energies extracted from fits to optical spectra of the widely studied CP47 antenna complex of photosystem II from spinach, though many general comments apply to other PSCs as well. Correct values of [Formula: see text] for chlorophyll (Chl) a in CP47 are essential for understanding its excitonic structure, population dynamics, and excitation energy pathway(s). To demonstrate this, we present a case study where simultaneous fits of multiple spectra (absorption, emission, circular dichroism, and nonresonant hole-burned spectra) show that several sets of parameters can fit the spectra very well. Importantly, we show that variable emission maxima (690-695 nm) and sample-dependent bleaching in nonresonant hole-burning spectra reported in literature could be explained, assuming that many previously studied CP47 samples were a mixture of intact and destabilized proteins. It appears that the destabilized subpopulation of CP47 complexes could feature a weakened hydrogen bond between the 13(1)-keto group of Chl29 and the PsbH protein subunit, though other possibilities cannot be entirely excluded, as discussed in this work. Possible implications of our findings are briefly discussed.

我们将重点放在光合复合体(psc)的位能解析问题上[公式:见文本],以便对文献中传播的相互矛盾的估计提出一些真正的关注。作为一个例子,我们提供了一个严格的评估,从菠菜光系统II的CP47天线复合体的光谱中提取的位置能量,尽管许多一般性的评论也适用于其他psc。CP47中叶绿素(Chl) a的正确值对于理解其激子结构、种群动态和激发能途径至关重要。为了证明这一点,我们提出了一个同时拟合多个光谱(吸收、发射、圆二色性和非共振孔烧光谱)的案例研究,表明几组参数可以很好地拟合光谱。重要的是,我们发现文献中报道的非共振孔燃烧光谱中的可变发射最大值(690-695 nm)和样品依赖漂白可以解释,假设许多先前研究的CP47样品是完整和不稳定蛋白质的混合物。似乎不稳定的CP47复合物亚群可能具有Chl29的13(1)-酮基团和pshh蛋白亚基之间的氢键减弱的特征,尽管其他可能性不能完全排除,正如本工作所讨论的那样。简要讨论了我们的研究结果可能产生的影响。
{"title":"On the Conflicting Estimations of Pigment Site Energies in Photosynthetic Complexes: A Case Study of the CP47 Complex.","authors":"Tonu Reinot,&nbsp;Jinhai Chen,&nbsp;Adam Kell,&nbsp;Mahboobe Jassas,&nbsp;Kevin C Robben,&nbsp;Valter Zazubovich,&nbsp;Ryszard Jankowiak","doi":"10.4137/ACI.S32151","DOIUrl":"https://doi.org/10.4137/ACI.S32151","url":null,"abstract":"<p><p>We focus on problems with elucidation of site energies [Formula: see text] for photosynthetic complexes (PSCs) in order to raise some genuine concern regarding the conflicting estimations propagating in the literature. As an example, we provide a stern assessment of the site energies extracted from fits to optical spectra of the widely studied CP47 antenna complex of photosystem II from spinach, though many general comments apply to other PSCs as well. Correct values of [Formula: see text] for chlorophyll (Chl) a in CP47 are essential for understanding its excitonic structure, population dynamics, and excitation energy pathway(s). To demonstrate this, we present a case study where simultaneous fits of multiple spectra (absorption, emission, circular dichroism, and nonresonant hole-burned spectra) show that several sets of parameters can fit the spectra very well. Importantly, we show that variable emission maxima (690-695 nm) and sample-dependent bleaching in nonresonant hole-burning spectra reported in literature could be explained, assuming that many previously studied CP47 samples were a mixture of intact and destabilized proteins. It appears that the destabilized subpopulation of CP47 complexes could feature a weakened hydrogen bond between the 13(1)-keto group of Chl29 and the PsbH protein subunit, though other possibilities cannot be entirely excluded, as discussed in this work. Possible implications of our findings are briefly discussed. </p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-06-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4137/ACI.S32151","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34452744","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 12
Removal of 4-Nitrophenol from Water Using Ag-N-P-Tridoped TiO2 by Photocatalytic Oxidation Technique. ag - n - p -三掺杂TiO2光催化氧化法去除水中4-硝基苯酚
Pub Date : 2016-04-04 eCollection Date: 2016-01-01 DOI: 10.4137/ACI.S31508
Temesgen Achamo, O P Yadav

Photocatalytic oxidation using semiconductor nanoparticles is an efficient, eco-friendly, and cost-effective process for the removal of organic pollutants, such as dyes, pesticides, phenols, and their derivatives in water. In the present study, nanosize Ag-N-P-tridoped titanium(IV) oxide (TiO2) was prepared by using sol-gel-synthesized Ag-doped TiO2 and soybean (Glycine max) or chickpea (Cicer arietinum) seeds as nonmetallic bioprecursors. As-synthesized photocatalysts were characterized using X-ray diffraction, Fourier transform infrared, and ultra violet (UV)-visible spectroscopic techniques. Average crystallite size of the studied photocatalysts was within 39-46 nm. Whereas doped Ag in TiO2 minimized the photogenerated electron-hole recombination, doped N and P extended its photoabsorption edge to visible region. Tridoping of Ag, N, and P in TiO2 exhibited synergetic effect toward enhancing its photocatalytic degradation of 4-nitrophenol (4-NP), separately, under UV and visible irradiations. At three hours, degradations of 4-NP over Ag-N-P-tridoped TiO2 under UV and visible radiations were 73.8 and 98.1%, respectively.

利用半导体纳米颗粒进行光催化氧化是一种高效、环保、经济的去除水中有机污染物的方法,如染料、农药、酚类及其衍生物。本研究以溶胶-凝胶法合成ag掺杂TiO2,以大豆(Glycine max)或鹰嘴豆(Cicer arietinum)种子为非金属生物递质制备纳米ag - n - p掺杂氧化钛(TiO2)。利用x射线衍射、傅里叶变换红外和紫外可见光谱技术对合成的光催化剂进行了表征。所研究的光催化剂的平均晶粒尺寸在39 ~ 46 nm之间。在TiO2中掺杂Ag使光生电子-空穴复合最小化,而掺杂N和P使TiO2的光吸收边缘扩展到可见光区。在紫外和可见光照射下,TiO2中Ag、N和P的三掺杂表现出协同作用,分别增强了TiO2对4-硝基苯酚(4-NP)的光催化降解。在紫外和可见光辐射下,4-NP对ag - n - p -三掺杂TiO2的降解率分别为73.8%和98.1%。
{"title":"Removal of 4-Nitrophenol from Water Using Ag-N-P-Tridoped TiO2 by Photocatalytic Oxidation Technique.","authors":"Temesgen Achamo,&nbsp;O P Yadav","doi":"10.4137/ACI.S31508","DOIUrl":"https://doi.org/10.4137/ACI.S31508","url":null,"abstract":"<p><p>Photocatalytic oxidation using semiconductor nanoparticles is an efficient, eco-friendly, and cost-effective process for the removal of organic pollutants, such as dyes, pesticides, phenols, and their derivatives in water. In the present study, nanosize Ag-N-P-tridoped titanium(IV) oxide (TiO2) was prepared by using sol-gel-synthesized Ag-doped TiO2 and soybean (Glycine max) or chickpea (Cicer arietinum) seeds as nonmetallic bioprecursors. As-synthesized photocatalysts were characterized using X-ray diffraction, Fourier transform infrared, and ultra violet (UV)-visible spectroscopic techniques. Average crystallite size of the studied photocatalysts was within 39-46 nm. Whereas doped Ag in TiO2 minimized the photogenerated electron-hole recombination, doped N and P extended its photoabsorption edge to visible region. Tridoping of Ag, N, and P in TiO2 exhibited synergetic effect toward enhancing its photocatalytic degradation of 4-nitrophenol (4-NP), separately, under UV and visible irradiations. At three hours, degradations of 4-NP over Ag-N-P-tridoped TiO2 under UV and visible radiations were 73.8 and 98.1%, respectively. </p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.4137/ACI.S31508","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"34404738","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 13
Quality Issues of Research Antibodies. 研究抗体的质量问题。
Pub Date : 2016-03-20 eCollection Date: 2016-01-01 DOI: 10.4137/ACI.S31614
Michael G Weller

According to several recent studies, an unexpectedly high number of landmark papers seem to be not reproducible by independent laboratories. Nontherapeutic antibodies used for research, diagnostic, food analytical, environmental, and other purposes play a significant role in this matter. Although some papers have been published offering suggestions to improve the situation, they do not seem to be comprehensive enough to cover the full complexity of this issue. In addition, no obvious improvements could be noticed in the field as yet. This article tries to consolidate the remarkable variety of conclusions and suggested activities into a more coherent conception. It is concluded that funding agencies and journal publishers need to take first and immediate measures to resolve these problems and lead the way to a more sustainable way of bioanalytical research, on which all can rely with confidence.

根据最近的几项研究,出乎意料的是,大量具有里程碑意义的论文似乎无法在独立实验室中重复。用于研究、诊断、食品分析、环境和其他目的的非治疗性抗体在这一问题上扮演着重要角色。虽然已经有一些论文提出了改进建议,但似乎还不够全面,无法涵盖这一问题的全部复杂性。此外,在这一领域尚未发现明显的改进。本文试图将各种不同的结论和活动建议整合成一个更加一致的概念。结论是,资助机构和期刊出版商需要立即采取首要措施解决这些问题,并引领生物分析研究走向更可持续的道路,让所有人都能放心地依赖这种研究。
{"title":"Quality Issues of Research Antibodies.","authors":"Michael G Weller","doi":"10.4137/ACI.S31614","DOIUrl":"10.4137/ACI.S31614","url":null,"abstract":"<p><p>According to several recent studies, an unexpectedly high number of landmark papers seem to be not reproducible by independent laboratories. Nontherapeutic antibodies used for research, diagnostic, food analytical, environmental, and other purposes play a significant role in this matter. Although some papers have been published offering suggestions to improve the situation, they do not seem to be comprehensive enough to cover the full complexity of this issue. In addition, no obvious improvements could be noticed in the field as yet. This article tries to consolidate the remarkable variety of conclusions and suggested activities into a more coherent conception. It is concluded that funding agencies and journal publishers need to take first and immediate measures to resolve these problems and lead the way to a more sustainable way of bioanalytical research, on which all can rely with confidence. </p>","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4803150/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85304225","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Development and Validation of Stability-Indicating RP-HPLC Method for Simultaneous Determination of Metformin HCl and Glimepiride in Fixed-Dose Combination 稳定指示反相高效液相色谱法同时测定盐酸二甲双胍和格列美脲的含量
Pub Date : 2016-03-13 DOI: 10.4137/ACI.S38137
Pradnya N. Vaingankar, P. Amin
A simple reversed-phase high-performance liquid chromatography method was developed and validated for simultaneous determination of Metformin hydrochloride (MET) and Glimepiride (GLM) in combination and estimation of their principal degradation products. The separation was achieved using JASCO Finepak SIL (250 mm × 4.6 mm i.d. 5 μm) at ambient temperature. The optimized mobile phase composed of an aqueous phase (20 mM phosphate buffer, adjusted to pH 3.0) and an organic phase (methanol:acetonitrile; 62.5:37.5) in the ratio of 80:20. The flow rate was 1 mL/minute, and the analytes were detected at 230 nm. The developed method was validated for accuracy, precision, specificity, linearity, and sensitivity. The chromatographic analysis time was approximately six minutes with the complete resolution of MET (Rt = 2.75 minutes) and GLM (Rt = 5.87 minutes). The method exhibited good linearity over the range of 5–30 μg/mL for MET and 1–10 μg/mL for GLM. The drugs in combination were subjected to various stress degradation studies as per the International Conference Harmonization (ICH) guidelines. Results obtained from the stress degradation studies revealed that the developed method is applicable for stability studies.
建立了一种简便的反相高效液相色谱法,用于同时测定盐酸二甲双胍(MET)和格列美脲(GLM)的主要降解产物。采用JASCO Finepak SIL (250 mm × 4.6 mm i.d. 5 μm)在常温下进行分离。优化后的流动相由水相(20 mM磷酸盐缓冲液,调节pH为3.0)和有机相(甲醇:乙腈;62.5:37.5),比例为80:20。流速为1 mL/min,检测波长为230 nm。验证了该方法的准确性、精密度、特异性、线性度和灵敏度。色谱分析时间约为6分钟,MET (Rt = 2.75分钟)和GLM (Rt = 5.87分钟)完全分辨。该方法在5 ~ 30 μg/mL和1 ~ 10 μg/mL范围内线性良好。根据国际会议协调(ICH)指南,这些药物组合受到各种压力降解研究。应力退化研究结果表明,所建立的方法适用于稳定性研究。
{"title":"Development and Validation of Stability-Indicating RP-HPLC Method for Simultaneous Determination of Metformin HCl and Glimepiride in Fixed-Dose Combination","authors":"Pradnya N. Vaingankar, P. Amin","doi":"10.4137/ACI.S38137","DOIUrl":"https://doi.org/10.4137/ACI.S38137","url":null,"abstract":"A simple reversed-phase high-performance liquid chromatography method was developed and validated for simultaneous determination of Metformin hydrochloride (MET) and Glimepiride (GLM) in combination and estimation of their principal degradation products. The separation was achieved using JASCO Finepak SIL (250 mm × 4.6 mm i.d. 5 μm) at ambient temperature. The optimized mobile phase composed of an aqueous phase (20 mM phosphate buffer, adjusted to pH 3.0) and an organic phase (methanol:acetonitrile; 62.5:37.5) in the ratio of 80:20. The flow rate was 1 mL/minute, and the analytes were detected at 230 nm. The developed method was validated for accuracy, precision, specificity, linearity, and sensitivity. The chromatographic analysis time was approximately six minutes with the complete resolution of MET (Rt = 2.75 minutes) and GLM (Rt = 5.87 minutes). The method exhibited good linearity over the range of 5–30 μg/mL for MET and 1–10 μg/mL for GLM. The drugs in combination were subjected to various stress degradation studies as per the International Conference Harmonization (ICH) guidelines. Results obtained from the stress degradation studies revealed that the developed method is applicable for stability studies.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77441406","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: 12
Electrochemical Behavior and Voltammetric Determination of a Manganese(II) Complex at a Carbon Paste Electrode 锰(II)配合物在碳糊电极上的电化学行为和伏安测定
Pub Date : 2016-01-18 DOI: 10.4137/ACI.S32150
Sophia Karastogianni, S. Girousi
Investigation of the electrochemical behavior using cyclic voltammetry and detection of [Mn2+(thiophenyl-2-carboxylic acid)2 (triethanolamine)] with adsorptive stripping differential pulse voltammetry. The electrochemical behavior of a manganese(II) complex [Mn2+(thiophenyl-2-carboxylic acid)2(triethanolamine)] (A) was investigated using cyclic and differential pulse voltammetry in an acetate buffer of pH 4.6 at a carbon paste electrode. Further, an oxidation–reduction mechanism was proposed. Meanwhile, an adsorptive stripping differential pulse voltammetric method was developed for the determination of manganese(II) complex.
循环伏安法研究电化学行为及吸附溶出差分脉冲伏安法检测[Mn2+(噻吩-2-羧酸)2(三乙醇胺)]。采用循环脉冲伏安法和差分脉冲伏安法研究了锰(II)配合物[Mn2+(噻吩-2-羧酸)2(三乙醇胺)](a)在pH为4.6的醋酸缓冲液中和碳膏电极上的电化学行为。进一步提出了氧化还原机理。同时,建立了吸附溶出差分脉冲伏安法测定锰(II)配合物的方法。
{"title":"Electrochemical Behavior and Voltammetric Determination of a Manganese(II) Complex at a Carbon Paste Electrode","authors":"Sophia Karastogianni, S. Girousi","doi":"10.4137/ACI.S32150","DOIUrl":"https://doi.org/10.4137/ACI.S32150","url":null,"abstract":"Investigation of the electrochemical behavior using cyclic voltammetry and detection of [Mn2+(thiophenyl-2-carboxylic acid)2 (triethanolamine)] with adsorptive stripping differential pulse voltammetry. The electrochemical behavior of a manganese(II) complex [Mn2+(thiophenyl-2-carboxylic acid)2(triethanolamine)] (A) was investigated using cyclic and differential pulse voltammetry in an acetate buffer of pH 4.6 at a carbon paste electrode. Further, an oxidation–reduction mechanism was proposed. Meanwhile, an adsorptive stripping differential pulse voltammetric method was developed for the determination of manganese(II) complex.","PeriodicalId":7781,"journal":{"name":"Analytical Chemistry Insights","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2016-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89746139","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: 7
期刊
Analytical Chemistry Insights
全部 Acc. Chem. Res. ACS Applied Bio Materials ACS Appl. Electron. Mater. ACS Appl. Energy Mater. ACS Appl. Mater. Interfaces ACS Appl. Nano Mater. ACS Appl. Polym. Mater. ACS BIOMATER-SCI ENG ACS Catal. ACS Cent. Sci. ACS Chem. Biol. ACS Chemical Health & Safety ACS Chem. Neurosci. ACS Comb. Sci. ACS Earth Space Chem. ACS Energy Lett. ACS Infect. Dis. ACS Macro Lett. ACS Mater. Lett. ACS Med. Chem. Lett. ACS Nano ACS Omega ACS Photonics ACS Sens. ACS Sustainable Chem. Eng. ACS Synth. Biol. Anal. Chem. BIOCHEMISTRY-US Bioconjugate Chem. BIOMACROMOLECULES Chem. Res. Toxicol. Chem. Rev. Chem. Mater. CRYST GROWTH DES ENERG FUEL Environ. Sci. Technol. Environ. Sci. Technol. Lett. Eur. J. Inorg. Chem. IND ENG CHEM RES Inorg. Chem. J. Agric. Food. Chem. J. Chem. Eng. Data J. Chem. Educ. J. Chem. Inf. Model. J. Chem. Theory Comput. J. Med. Chem. J. Nat. Prod. J PROTEOME RES J. Am. Chem. Soc. LANGMUIR MACROMOLECULES Mol. Pharmaceutics Nano Lett. Org. Lett. ORG PROCESS RES DEV ORGANOMETALLICS J. Org. Chem. J. Phys. Chem. J. Phys. Chem. A J. Phys. Chem. B J. Phys. Chem. C J. Phys. Chem. Lett. Analyst Anal. Methods Biomater. Sci. Catal. Sci. Technol. Chem. Commun. Chem. Soc. Rev. CHEM EDUC RES PRACT CRYSTENGCOMM Dalton Trans. Energy Environ. Sci. ENVIRON SCI-NANO ENVIRON SCI-PROC IMP ENVIRON SCI-WAT RES Faraday Discuss. Food Funct. Green Chem. Inorg. Chem. Front. Integr. Biol. J. Anal. At. Spectrom. J. Mater. Chem. A J. Mater. Chem. B J. Mater. Chem. C Lab Chip Mater. Chem. Front. Mater. Horiz. MEDCHEMCOMM Metallomics Mol. Biosyst. Mol. Syst. Des. Eng. Nanoscale Nanoscale Horiz. Nat. Prod. Rep. New J. Chem. Org. Biomol. Chem. Org. Chem. Front. PHOTOCH PHOTOBIO SCI PCCP Polym. Chem.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
0
微信
客服QQ
Book学术公众号 扫码关注我们
反馈
×
意见反馈
请填写您的意见或建议
请填写您的手机或邮箱
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
现在去查看 取消
×
提示
确定
Book学术官方微信
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术
文献互助 智能选刊 最新文献 互助须知 联系我们:info@booksci.cn
Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。
Copyright © 2023 Book学术 All rights reserved.
ghs 京公网安备 11010802042870号 京ICP备2023020795号-1