Determination of carbamazepine and its impurities iminostilbene and iminodibenzyl in solid dosage form by column high-performance liquid chromatography

An accurate and precise RP-HPLC method was developed and validated for the determination of carbamazepine and its impurities iminostilbene and iminodibenzyl in a tablet formulation with fluphenazine as an internal standard. Buffer-methanol (50 + 50, v/v) was used as the mobile phase. During validation, specificity, linearity, precision, accuracy, LOD, LOQ, and robustness of the method were tested. The method was proven to be specific against placebo interference. Linearity was evaluated over the concentration range of 100-500, 0.05-0.25, and 0.1-0.5 microg/mL, and the r values were 0.9994, 0.9997, and 0.9979 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Intraday precision of the method was good, and RSD was below 2% for all analytes. The accuracy of the method ranged from 100.69 to 102.10, 99.76 to 102.66, and 99.26 to 100.08% for carbamazepine, iminostilbene, and iminodibenzyl, respectively. LOD was 0.0125, 0.025, and 0.05 microg/mL and LOQ was 0.05, 0.05, and 0.1 microg/mL for carbamazepine, iminostilbene, and iminodibenzyl, respectiviely. Robustness of the method was proven by using a chemometric approach. The method was successfully applied to the analysis of commercially available carbamazepine tablets and showed good repeatability, with RSD below 2%.     

前列舒通胶囊中26种无机元素的分析

目的：明确造成前列舒通胶囊不同批次间差异的标志性无机元素,并进行安全性评价。方法：采用ICP-MS测定制剂中Al、As、B、Ba、Ca、Cd、Co、Cr、Cu、Fe、K、Mg、Mn、Mo、Na、Ni、Pb、Sb、Se、Sn、Sr、Ti、Tl、V、Zn和Hg元素含量并进行数据分析。运用主成分及综合评分结合聚类分析手段,确定制剂的特征性元素;进行元素含量和相关性分析,明确不同批次各元素的差异及元素之间的关系;以多元素含量为指标,绘制无机元素谱图。结果：19批样品中均未检测出Se、Mo、Sn、Sb、Tl和Hg,且Pb、Cd、As、Cu、Hg均符合限量标准,无机元素含量谱图趋势一致。主成分分析提取了4个主成分,确定元素B、K、Al、V、Cr、Ca、Ti、Na、Co和Mn可作为特征元素。主成分得分图将19批样品分为两类,聚类分析及综合评分结果与其一致,两类样品中各元素含量存在差异性。相关性分析中,明确了B与K、Al、Cr正相关,K与Cr、Co正相关,V与Cr、Mn正相关,Mn与Co正相关,Ca、Ti、Na两两正相关。结论：通过分析前列舒通胶囊中无机元素含量,确定了特征元素,为前列舒通胶囊质量全面控制研究提供科学依据。     

A Festschrift in honor of Akira Imamura��s 77th birthday, his recent retirement, and his many contributions to theoretical chemistry

The Imamura Festschrift Issue of Theoretical Chemistry Accounts is a special multifocus international issue commemorating the 77th birthday of Professor Akira Imamura and his many contributions to the fields of theoretical chemistry, polymer science, molecular biophysics, chemical physics, and molecular biology. This issue has contributions in theoretical developments of methods applicable to larger polymeric systems, for example, the elongation method pioneered by Professor Imamura and his group, and more recently by the groups of Professor Yuriko Aoki at Kyushu University and Professor Feng Long Gu at South China Normal University, supported by several funds from the Japan Science and Technology Agency (JST). In addition, there are contributions from top experimental and theoretical groups in the areas of nanotechnology, bionanotechnology, quantum transport theory, molecular biophysics, molecular electronics, and even molecular medicine and medical diagnostics, where the marriage between theory and experiment is very important to be able to fully understand, interpret, and utilize the wealth of new and exciting experimental data. The development of new and refined methods, and the extension of older more conventional methods, will be required for these fields to continue to evolve/co-evolve and develop, as they have in the last 60?years. But to evolve in a guided fashion (guided evolution), that is, to meet the needs and functions of not only the individual scientists and research groups but also of society in general, will require a concerted effort from not only experimentalists and theoreticians in each individual subdiscipline but also for them to work together and share their accumulated knowledge and experience, as is now being done in various research networks around the world, including the one originally initiated/formed by Professor Imamura and Professor Janos Ladik at the Third International Congress of Quantum Chemistry (ICQC) in Kyoto, Japan. Through this network, Professor Imamura has been able to pass on a wealth of knowledge, expertise, and experience to the current and future generations of scientists in Germany, the United States, and China, as Professor Imamura is still doing with his lectures both in Japan at Kyushu University and in China at South China Normal University, and previously in Erlangen at the University of Erlangen, in Heidelberg at the German Cancer Research Center (DKFZ) in Germany, and in Ithaca, New York at Cornell University in the United States. He has been a real example of the modern protean research scientist and professor who has continued to be in research and teaching, active well beyond the formerly set retirement age of 63 or 65 set by society. The idea that researchers and professors cannot be active in their 60s, 70s, and 80s has now also been shown to be a misconception that needs to be corrected at the funding and institutional levels. Too many very active, knowledgeable, and experienced researchers and professors have been forced to stand on the sidelines, while those who have replaced them have very little practical knowledge, expertise, and more importantly, life experience. A whole generation of young academics are being hired who have never worked a day in industry, never visited an industrial laboratory and/or research group, and hence are unable, (don??t know) and in many cases, unwilling to train and educate their students with the skills they need to not only work in industry but also to create new and exciting new industries. The idea that the large chemical and pharmaceutical companies and government laboartories will hire all of the ever increasing numbers of undergraduate and graduate (MSc and PhD) students no longer applies. The university mission is no longer just to teach, give knowledge, and to do research, but also to innovate, that is, to train the students to take their acquired knowledge from their text books and apply it with the newly acquired knowledge in the research laboratories to start and develop new industries and companies. But this means that the students need to be trained in the fields of engineering economics, finance, and scientific and international law, so that they are able to undertake such projects, in addition to understanding and applying their scientific knowledge. It will also require a concerted effort by funding agencies, state, local, federal, and even international bodies that seek to create and sustain strong economies and infrastructure, which will support and be supported by the highly motivated, trained, and educated work forces. The third pillar is now being established, but it needs to now be totally and completely integrated with the other establishments and infrastructure.     

Environmentally Friendly Techniques and Their Comparison in the Extraction of Natural Antioxidants from Green Tea,Rosemary, Clove,and Oregano

Many current food and health trends demand the use of more ecological, sustainable, and environmentally friendly techniques for the extraction of bioactive compounds, including antioxidants. However, extraction yields and final antioxidant activities vary between sources and are highly influenced by the given extraction method and nature and ratio of the employed solvent, especially for total polyphenols, flavonoids, and anthocyanins, which are well recognized as natural antioxidants with food applications. This review focused on the most common extraction techniques and potential antioxidant activity in the food industry for various natural antioxidant sources, such as green tea, rosemary, clove, and oregano. Green extraction techniques have been proven to be far more efficient, environmentally friendly, and economical. In general, these techniques include the use of microwaves, ultrasound, high hydrostatic pressure, pulsed electric fields, enzymes, and deep eutectic solvents, among others. These extraction methods are described here, including their advantages, disadvantages, and applications.     

Ziziphora clinopodioides Lam leaf aqueous extract mediated novel green synthesis of iron nanoparticles and its anti-hemolytic anemia potential: A chemobiological study

In this study, the aqueous extract Ziziphora clinopodioides was used to biosynthesis of iron nanoparticles. A green, productive, and environmentally method was developed for the valuable study and the effective preparation of the green-synthesis of iron nanoparticles using aqueous extracts from the leaf of Ziziphora clinopodioides as a result of reducing and stabilizing factor. The simplicity of the synthesis procedures and easy work up are the benefits of the present study. The structural and morphological characterization of green‐synthesized FeNPs was performed by Uv–Vis. and FT-IR spectroscopy, XRD, SEM, and EDX techniques. The SEM images have exhibited an equal and uniform spherical morphology in size of 30.04. We also investigated the anti-hemolytic anemia property of FeNPs in an animal model of hemolytic anemia. In vivo assay, induction of hemolytic anemia was done by phenylhydrazine in mice. FeNPs significantly reduced the weight and volume of liver and spleen and the concentration of pro-inflammatory cytokines and increased the body weight, the anti-inflammatory cytokines concentration, and the total platelet, WBC, neutrophil, lymphocyte, eosinophil, monocyte, and basophil counts, and RBC parameters as compared to the untreated mice. About the biochemical parameters, FeNPs significantly increased GPx, CAT, and SOD in serum, liver, and spleen, and also HDL, total protein, and albumin in serum, and decreased GR in serum, liver, and spleen, and also erythropoietin, ferritin, ferrous, creatinine, urea, LDL, triglyceride, cholesterol, GGT, ALT, AST, and ALP in serum as compared to the anemic mice. DPPH test revealed similar antioxidant potentials for FeNPs and Butylated hydroxytoluene. FeNPs had low cell viability dose-dependently against HUVEC cell line. It appears that FeNPs can be administrated as a hematoprotective and anti-hemolytic anemia drug or supplement for the treatment of hemolytic anemia in the clinical trial.     

Synthesis,structure, and function of internally functionalized dendrimers

The past three decades have witnessed an exponential increase in the structural diversity and applications of dendrimers, spanning across drug delivery and diagnostics, protein, and enzyme mimicry, solubility enhancement, coatings, light harvesting, and catalysis. The dendrimer community has recently focused on internally functionalized dendrimers (IFDs) owing to their advanced design and functionality. The synthesis of IFDs relies on advanced orthogonal chemistries and/or (de)protection schemes, as well as careful purification to minimize polydispersity of composition and molecular weight. The studies published on IFDs, however, lay scattered across the chemical literature, and a comprehensive presentation of structural rationale, synthetic procedures, and technologically relevant applications is missing. To address this need, this review presents a comprehensive collection and discussion of all available studies on IFDs, detailing their methods of synthesis and their structure–function correlations. The wide variety of internal functionalities, including hydroxyl, amine, carboxylic acid, allyl, alkyne, and imidazole groups, enables myriad applications in biochemistry, chemical and biomedical engineering, and material science. Particular focus is given to IFDs that are amenable to modular synthetic strategies, which promote higher synthetic yield and scalability, and therefore possess stronger translational and commercial potential. As such, this review guides research groups pursuing the difficult task of IFD rational design and synthesis providing them a concise roadmap to their mission.     

含8-羟基喹啉侧基聚酯及其锌、铝配合物的合成和性能

合成了2种新型含8-羟基喹啉侧基聚酯(P5,P6),进一步与无水醋酸锌和六水氯化铝反应,得到4种聚酯锌、铝配合物(P5-Zn,P6-Zn,P5-Al,P6-Al)。采用元素分析仪、傅里叶变换红外光谱仪、紫外可见光谱仪、核磁共振氢谱仪、凝胶渗透色谱仪、热重分析仪和荧光光谱仪等技术手段对其结构和性能进行了表征。聚酯P5和P6易溶于四氢呋喃(THF)、N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAC)、二甲基亚砜(DMSO)和N-甲基吡咯烷酮(NMP)等常用的有机溶剂,配合物P5-Zn、P6-Zn、P5-Al和P6-Al部分溶于DMF、DMAC、DMSO和NMP等溶剂。聚酯P5和P6的质均相对分子质量Mw为4.11×10~4和5.42×10~4,相对分子质量分布指数PDI为1.50和1.40。聚酯P5和P6的5%失重温度分别为261.4和291.1℃,配合物P5-Zn、P6-Zn、P5-Al和P6-Al的5%失重温度分别为307.7、306.2、286.3和297.8℃。聚酯P5和P6的DMF溶液(5×10-5 mol/L)在432和429nm处发射较弱紫色荧光,配合物P5-Zn、P6-Zn、P5-Al和P6-Al的DMF溶液(5×10~(-5) mol/L)分别在540、537、517和522nm处发强绿色荧光,固体分别在550、556、531和535nm处发射强绿色荧光。     

Self-aggregation of ionic C(10) surfactants having different headgroups with special reference to the behavior of decyltrimethylammonium bromide in different salt environments: a calorimetric study with energetic analysis

Self-aggregation of C10 ionic surfactants with different head groups, viz., decylpyridinium chloride, sodium decylsulfate, decylammonium bromide, decyldimethylammonium bromide, and decyltrimethylammonium bromide, was studied in the aqueous medium by microcalorimetric and conductometric methods. The effects of temperature and different salts (NaF, NaCl, NaBr, NaI, Na2SO4, Na2S2O7, Na-benzoate, and Na-salicylate) were also studied on decyltrimethylammonium bromide representatives. The cmc, counterion binding, and energetics of micellization were evaluated and discussed. The energetic parameters, enthalpy, entropy, and specific heat of micellization obtained from direct calorimetry and the indirect van't Hoff method were compared and discussed.     

高效液相色谱-串联质谱法快速同时测定土壤中草甘膦、草铵膦及其代谢物

建立了快速同时测定土壤中草甘膦(GLY)、草铵膦(GLUF)及其代谢物的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法.分别对前处理和色谱-质谱条件进行优化,样品采用0.5 mol/L氨水作为溶剂振荡提取,离心,上清液过滤膜后,直接采用HPLC-MS/MS测定,电喷雾离子源(ESI-),多反应监测(MRM)模式...     

Population genetics and forensic efficiency of twenty‐one novel microsatellite loci of Chinese Yi ethnic group

In this study, we investigated polymorphic distributions of allelic frequencies and forensic genetic parameters of 21 novel autosomal microsatellite loci from 110 unrelated healthy individuals of Chinese Yi ethnic group. Expected heterozygosity, power of discrimination, and polymorphic information content ranged from 0.617 to 0.812, 0.777 to 0.936 and 0.560 to 0.790. The microsatellite loci showed high forensic efficiency. The total discrimination power and cumulate probability of exclusion were 0.99999999999999999986902 and 0.999998818, respectively. Locus‐by‐locus allelic frequencies were compared using analysis of molecular variance (AMOVA) method, and the statistically significant differences were observed between Yi group and Russian, Tujia, Kazak, Bai, Ningxia Han, Salar, Tibetan, and Uigur groups at 5, 6, 7, 7, 7, 8, 12, and 13 loci, respectively. The results of genetic distance comparisons, genetic structure analyses, and principal component analysis all indicated that the Yi group showed relatively short genetic relationships with Russian, Salar, and Bai group. The experimental results showed that the 21 loci in the multiplex system provided highly polymorphic information and forensic efficiency for forensic individual identification and paternity testing, also basic population data for population genetics and anthropological research.     

Scrophulariae Radix: An Overview of Its Biological Activities and Nutraceutical and Pharmaceutical Applications

Scrophulariae Radix (SR) has an important role as a medicinal plant, the roots of which are recorded used to cure fever, swelling, constipation, pharyngitis, laryngitis, neuritis, sore throat, rheumatism, and arthritis in Asia for more than two thousand years. In this paper, the studies published on Scrophularia buergeriana (SB) and Scrophularia ningpoensis (SN) in the latest 20 years were reviewed, and the biological activities of SB and SN were evaluated based on in vitro and in vivo studies. SB presented anti-inflammatory activities, immune-enhancing effects, bone disorder prevention activity, neuroprotective effect, anti-amnesic effect, and anti-allergic effect; SN showed a neuroprotective effect, anti-apoptotic effect, anti-amnesic effect, and anti-depressant effect; and SR exhibited an immune-enhancing effect and cardioprotective effects through in vitro and in vivo experiments. SB and SN are both known to exert neuroprotective and anti-amensice effects. This review investigated their applicability in the nutraceutical, functional foods, and pharmaceutical industries. Further studies, such as toxicological studies and clinical trials, on the efficacy and safety of SR, including SB and SN, need to be conducted.     

Growth Parameter and Viability Modifications of Escherichia coli by Phenolic Compounds and Argentine Wine Extracts

The anti-bacterial effect of pure non-flavonoids gallic, vanillic, protocatechuic, and caffeic acids and flavonoids quercetin, rutin, and catechin and the effect of total polyphenols of three Argentinean wine varieties, Cabernet Sauvignon, Malbec, and Merlot, against Escherichia coli, microorganism frequently detected in fresh and processed foods, was investigated. The hydroxycinnamic derivate caffeic acid and the flavonoid quercetin were the more effective against E. coli. The polyphenol effect was ethanol independent. The E. coli decimal reduction times were 2.9, 2.1, and 0.65 h for Malbec wine and 2.8, 2.3, and 0.64 h for Merlot wine with respect to 1x, 2x, and 4x concentrated wine samples, respectively. For Cabernet Sauvignon wine, the values were 6.3, 3.7, and 1.28 h for 1x, 2x, and 4x concentrated samples, respectively. With clarified wines, the decimal reduction times were higher with values ranging from 15 to 18.4 h in the wine samples. So the phenolic compounds present in red wines could be considered as an interesting alternative to be used as natural preservative against pathogenic microorganisms.     

Simultaneous extraction and quantification of lamotrigine,phenobarbital, and phenytoin in human plasma and urine samples using solidified floating organic drop microextraction and high‐performance liquid chromatography

A novel and simple method based on solidified floating organic drop microextraction followed by high‐performance liquid chromatography with ultraviolet detection has been developed for simultaneous preconcentration and determination of phenobarbital, lamotrigine, and phenytoin in human plasma and urine samples. Factors affecting microextraction efficiency such as the type and volume of the extraction solvent, sample pH, extraction time, stirring rate, extraction temperature, ionic strength, and sample volume were optimized. Under the optimum conditions (i.e. extraction solvent, 1‐undecanol (40 μL); sample pH, 8.0; temperature, 25°C; stirring rate, 500 rpm; sample volume, 7 mL; potassium chloride concentration, 5% and extraction time, 50 min), the limits of detection for phenobarbital, lamotrigine, and phenytoin were 1.0, 0.1, and 0.3 μg/L, respectively. Also, the calibration curves for phenobarbital, lamotrigine, and phenytoin were linear in the concentration range of 2.0–300.0, 0.3–200.0, and 1.0–200.0 μg/L, respectively. The relative standard deviations for six replicate extractions and determinations of phenobarbital, lamotrigine, and phenytoin at 50 μg/L level were less than 4.6%. The method was successfully applied to determine phenobarbital, lamotrigine, and phenytoin in plasma and urine samples.     

Chromatographic Determination of Lignans (Antioxidants) in Food Products

Interest in lignans is continually growing in recent years because of their strong antioxidant properties and other biological characteristics, positively affecting human health. Methods for the extraction, identification, and determination of lignans are developed; lignan species and their quantity in food products are determined, and databases of lignans in food products have been created in several countries (Finland, Netherlands, United States, Canada, United Kingdom, Japan, and Spain). In this review, we consider chromatographic methods (gas, liquid, supercritical fluid, and thin-layer chromatography) used to identify and determine natural lignans and isolate them in an individual state. Most natural lignans are found in flax and sesame seeds, cereals, some vegetables, fruits, and berries.     

Recent development in nanomaterials fabricated paper-based colorimetric and fluorescent sensors: A review

The paper-based sensing devices have drawn a broad interest in analytical chemistry for colorimetric and fluorescent-based analysis of biological, environmental, clinical, and food samples. It is due to the simple, rapid, biodegradable, user-friendly, less expensive, and low waste generation into the environment. Here, the recent development of paper-based sensors fabricated with different noble metal nanoparticles (NPs) and semiconductor and carbon quantum dots (QDs) is demonstrated to analyze several chemical substances from various samples. User-friendly and portable recording devices such as digital cameras, smartphones, scanners, etc. along with color detecting softwares are employed to measure the color intensity of nanomaterials fabricated paper devices after the deposition of a sample solution containing various chemical substances. The advantages and disadvantages of incorporating nanomaterials in the paper substrate (direct deposition, inkjet printing, screen printing and wax printing) are illustrated. The mechanism for colorimetric, fluorescence, phosphorescence, and chemiluminescence sensing using noble metal NPs (Ag, Cu, and Au), semiconductors, and carbon QDs for the determination of metal ions, anions, pesticides, biomolecules, and other toxic chemical substances are discussed. Thus, this review article would be highly useful for scientists and researchers to design colorimetric sensors to monitor chemical toxicants in clinical, environment, foods, and many other related samples.     

Novel syntheses of hexahydro-1H-pyrrolo[1,2-a]ĭmidazoles and Octahydroimidazo[1,2-a]pyridines

1-Phenyl-5-(benzotriazol-1-yl)hexahydro-1H-pyrrolo[1,2-a]?midazole (18) and 1-phenyl-5-benzotriazolyloctahydroimidazo[1,2-a]pyridine (27) were readily prepared from succindialdehyde or glutaraldehyde, benzotriazole, and N-phenylethylenediamine. Synthons 18 and 27 reacted with Grignard reagents, allylsilanes, silyl ethers, and triethyl phosphite to produce 1-phenyl-5-substituted-hexahydro-1H-pyrrolo[1,2-a]?midazoles 20a-f, 22, 24a,b, and 25 and 1-phenyl-5-substituted-octahydroimidazo[1, 2-a]pyridines 28a-e, 32, 33a,b, and 34 in good to excellent yields. The configurations of 20, 22, 24, and 25 were determined to be cis isomers by NOE experiment, while the configurations and conformations of 28a-e, 32, 33a,b, and 34 were elucidated by (1)H-(1)H COSY and (1)H-(13)C COSY.     

Variable strategy toward carbasugars and relatives. 4. Viable access to (4a-carbapentofuranosyl)amines, (5a-carbahexopyranosyl)amines,and amino acids thereof

A chiral, divergent synthesis of two carbafuranosylamines, 1 and 2, two carbapyranosylamines, 3 and 4, two carbafuranosylamino acids, 5 and 6, and two carbapyranosylamino acids, 7 and 8, has been achieved. Highlights of the procedure include the following: a diastereoselective crossed vinylogous Mukaiyama aldol coupling between N-(tert-butoxycarbonyl)-2-[(tert-butyldimethylsilyl)oxy]pyrrole (TBSOP, 9) and 2,3-O-isopropylidene-D-glyceraldehyde (10) for the assembly of the target compound carbon backbone; a high-yielding silylative cycloaldolization that gives the cyclopentanoid and cyclohexanoid motifs; and a reductive or hydrolytic breakage of the lactam C(O)-N link to liberate the carbasugar and install the desired pseudo-anomeric amine and the hydroxymethyl or carboxyl functionalities. The sequences leading to trans-configured carbafuranosyl compounds 1 and 5 and carbapyranosyl compounds 3 and 7 were 12- and 13-step processes, with overall yields of 34%, 35%, 17%, and 16%. Cis-configured isomers 2, 4, 6, and 8 were obtained only in minor yields.     

中国微量元素研究二十年

综述了中国微量元素科学研究的现状、意义、存在问题及其对策。在研究现状方面,包括：环境与人(环境、活质与人体元素丰度的相关性,食品与营养,土壤与恶性肿瘤,环境与地方病),体内分布(脏器,胎儿,细胞,骨和晶状体),代谢和疾病(癌症,糖尿病,心血管病,高血压,痴呆症,其他疾病),健康和长寿(中药,长寿元素谱,健康饮用水),实验研究和生物学效应研究(延寿实验,抗癌实验,生物学效应研究),保健补剂和食疗产品(营养补充剂,功能性食品和食疗产品)。在重要意义方面,包括：国计民生的大事(土质恶化问题,地方病流行问题,有害物质的排放问题,重金属污染问题),健康长寿的保障(营养的评估和监督,疾病的筛选和诊断,顽症的预防和治疗),新学科的催生(元素平衡医学,微量元素营养生态学,中药元素学和头发元素学,元素平衡保健医学,元素医学地理学)。在存在问题方面,包括：对人体内外生态环境的整体性和系统性认识不足,对饮水中微量元素的作用认识不够,对血液和头发的本质认识不清,文献数据的不可比性和组织结构分散。几点建议,包括：成立国家级微量元素专家委员会,制订头发分析标准化方法,建立中国人体和中国总膳食全元素数据库,开展长寿成因调查,开展中国食用海藻全元素成分调查,以及研究和开发大众化元素平衡保健食品。