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  • 1.

    【2hr】Ten Basic Rules of Antibody Validation

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    机译 抗体验证的十个基本规则
    • 作者：Michael G Weller
    • 刊名：Analytical Chemistry Insights
    • 2018年第期
    摘要：The quality of research antibodies is an issue for decades. Although several papers have been published to improve the situation, their impact seems to be limited. This publication makes the effort to simplify the description of validation criteria in a way that the occasional antibody user is able to assess the validation level of an immunochemical reagent. A simple, 1-page checklist is supplied for the practical application of these criteria.
  • 2.

    【2hr】Chitosan Membrane Embedded With ZnO/CuO Nanocomposites for the Photodegradation of Fast Green Dye Under Artificial and Solar Irradiation

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    机译 嵌入ZnO / CuO纳米复合材料的壳聚糖膜在人工和太阳光照射下对速溶绿色染料的光降解
    • 作者：Eman Alzahrani
    • 刊名：Analytical Chemistry Insights
    • 2018年第期
    摘要：Fast Green (FCF) dye is commonly used in both cytology and histology applications. Previous studies have found that it can cause mutagenic and tumorigenic effects in experimental human and animal populations. It can also be a source of skin, eye, respiratory, and digestive irritation. The purpose of this study was to examine the use of thin film membranes to degrade FCF. A thin film membrane of chitosan (CS) was fabricated and subsequently filled with zinc oxide nanoparticles (ZnO) or ZnO/CuO-heterostructured nanocomposites. The CS membrane was used as a matrix, and the nanomaterials were used as photocatalysts. The prepared membranes were characterised by four analytical techniques: atomic force microscopy, scanning electron microscopy, X-ray diffraction, and energy-dispersive X-ray analyses. The photocatalytic activity of the fabricated membranes was evaluated by performing experiments in which aqueous solutions of FCF dye that contained the fabricated membrane were irradiated with solar light or UV light. The photodegradation percentage was spectrophotometrically determined by monitoring the maximum wavelengths (λmax) of FCF at 623 nm for different irradiation times. The decolourisation percentages of the dye under solar light were 57.90% and 60.23% using the CS-ZnO and CS-ZnO/CuO membranes, respectively. When UV light irradiation was employed as the source of irradiation, the photodegradation percentages of FCF were 71.45% and 91.21% using the CS-ZnO and CS-ZnO/CuO membranes, respectively. These results indicated that the best photocatalytic system for the degradation of FCF dye was CS-ZnO/CuO membrane in combination with UV light irradiation. The study also found that it was easy to separate the prepared membranes after the reaction without the need for a centrifuge or magnet. The results demonstrate the potential for CS-ZnO and CS-ZnO/CuO membranes for use as effective sorbents during the process of photodegradation of harmful dyes within waste water recycling practices.
  • 3.

    【2hr】Analytical Methods for the Determination of Mineral Oil Saturated Hydrocarbons (MOSH) and Mineral Oil Aromatic Hydrocarbons (MOAH)—A Short Review

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    机译 测定矿物油饱和烃（MOSH）和矿物油芳烃（MOAH）的分析方法—简述
    摘要：Mineral oils (such as paraffinum liquidum or white oil), which consist of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), are widely applied in various consumer products such as medicines and cosmetics. Contamination of food with mineral oil may occur by migration of mineral oil containing products from packaging materials, or during the food production process, as well as by environmental contamination during agricultural production. Considerable analytical interest was initiated by the potential adverse health effects, especially carcinogenic effects of some aromatic hydrocarbons. This article reviews the history of mineral oil analysis, starting with gravimetric and photometric methods, followed by on-line-coupled liquid chromatography with gas chromatography and flame ionization detection (LC-GC-FID), which still is considered as gold standard for MOSH-MOAH analysis. Comprehensive tables of applications in the fields of cosmetics, foods, food contact materials, and living organisms are provided. Further methods including GCxGC-MS methods are reviewed, which may be suitable for confirmation of LC-GC-FID results and identification of compound classes. As alternative to chromatography, nuclear magnetic resonance (NMR) spectroscopy has recently been suggested for MOSH-MOAH analysis, especially with the possibility of detecting only the toxicologically relevant aromatic rings. Furthermore, NMR may offer potential as rapid screening especially with low-field instruments usable for raw material control.
  • 4.

    【2hr】In Vitro Studies of the Antimicrobial and Free-Radical Scavenging Potentials of Silver Nanoparticles Biosynthesized From the Extract of Desmostachya bipinnata

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    机译 Desmostachya bipinnata提取物生物合成的银纳米粒子的抗菌和自由基清除潜力的体外研究。
    摘要：The aim of this study was to perform green synthesis of silver nanoparticles (AgNPs) from the leaf extract of Desmostachya bipinnata (Dharba), a medicinally important herb which is widely used across India. Synthesized AgNPs were analyzed by UV-Visible spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDAX). The results have confirmed that green synthesis of AgNPs leads to the fabrication of sphere-shaped particles with a diameter of 53 nm. Furthermore, these AgNPs were subjected to antioxidant and antimicrobial studies against gram-negative and gram-positive bacteria, where AgNPs at a concentration of 20 mg/mL showed highest zone of inhibition. Synthesized AgNPs were evaluated for their antioxidant activity by 1, 1-diphenyl-2-picryl hydrazyl radical (DPPH), H2O2, and superoxide inhibiting assays; increasing concentration has showed increase in scavenging ability. Cell toxicity was assessed on HepG2 cell lines, and synthesized nanoparticles at a concentration of 128 μg/mL produced significant reduction in viability of Hep cells (P < .05). The availability of Dharba throughout the year and the eco-friendly approach in the synthesis of AgNPs coupled with bioactivity has demonstrated its potential as a novel biomaterial which can be used for various biomedical applications.
  • 5.

    【2hr】An Accurate Assessment of Docosahexaenoic Acid in Laying Hen Serumfor Regulatory Studies

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    机译 产蛋血清中二十二碳六烯酸的准确评估用于法规研究
    摘要：Diets rich in omega-3 fatty acids (n-3 FA) have been associated with several health benefits. With the increased interest in n-3 FA both scientifically and societally, the accurate detection of such analytes has become increasingly important. Recently, tandem mass spectrometry (MS/MS) with electrospray ionization interface (ESI), hyphenated to both gas chromatography (GC) and liquid chromatography (LC), has become a valuable tool in the detection of docosahexaenoic acid (DHA). Liquid chromatography-electrospray ionization interface-tandem mass spectrometry methods have been developed for the determination of DHA in canine and poultry species. The objective of this article is to investigate whether LC-ESI-MS/MS is fit for purpose for the determination of DHA in laying hen serum. The disclosure of this work will be beneficial for researchers investigating poultry enrichment for regulatory and toxicological studies. The method was found to be linear over the range. Precision and accuracy results met acceptance criteria and the Limit of Quantitation (LOQ) was established as 1 µg/mL. Recoveries of DHA were obtained for quality control samples and stability studies were performed. The results of the verification study complimented those of the validation study. In summation,the method was established as fit for purpose for measuring total DHA in layinghen serum.
  • 6.

    【2hr】Colorimetric Detection Based on Localised Surface Plasmon Resonance Optical Characteristics for the Detection of Hydrogen Peroxide Using Acacia Gum–Stabilised Silver Nanoparticles

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    机译 基于本地表面等离子体共振光学特性的比色法检测相思胶稳定化的银纳米粒子检测过氧化氢
    • 作者：Eman Alzahrani
    • 刊名：Analytical Chemistry Insights
    • 2017年第期
    摘要：The use of nanoparticles in sensing is attracting the interest of many researchers. The aim of this work was to fabricate Acacia gum–stabilised silver nanoparticles (SNPs) using green chemistry to use them as a highly sensitive and cost-effective localised surface plasmon resonance (LSPR) colorimeter sensor for the determination of reactive oxygen species, such as hydrogen peroxide (H2O2). Silver nanoparticles were fabricated by the reduction of an inorganic precursor silver nitrate solution (AgNO3) using white sugar as the reducing reagent and Acacia gum as the stabilising reagent and a sonication bath to form uniform silver nanoparticles. The fabricated nanoparticles were characterised by visual observation, ultraviolet-visible (UV-Vis) spectrophotometry, transmission electron microscopy (TEM) analysis, energy-dispersive X-ray spectroscopy (EDAX), thermogravimetric analysis (TGA), and Fourier transform infrared spectroscopy (FT-IR). The TEM micrographs of the synthesised nanoparticles showed the presence of spherical nanoparticles with sizes of approximately 10 nm. The EDAX spectrum result confirmed the presence of silver (58%), carbon (30%), and oxygen (12%). Plasmon colorimetric sensing of H2O2 solution was investigated by introducing H2O2 solution into Acacia gum–capped SNP dispersion, and the change in the LSPR band in the UV-Vis region of spectra was monitored. In this study, it was found that the yellow colour of Acacia gum–stabilised SNPs gradually changed to transparent, and moreover, a remarkable change in the LSPR absorbance strength was observed. The calibration curve was linear over 0.1–0.00001 M H2O2, with a correlation estimation (R2) of .953. This was due to the aggregation of SNPs following introduction of the H2O2 solution. Furthermore, the fabricated SNPs were successfully used to detect H2O2 solution in a liquid milk sample, thereby demonstrating the ability of the fabricated SNPs to detect H2O2 solution in liquid milk samples. This work showed that Acacia gum–stabilised SNPs may have the potential as a colour indicator in medical and environmental applications.
  • 7.

    【2hr】Review of Current Applications of Immunohistochemistry in Pediatric Nonneoplastic Gastrointestinal, Hepatobiliary, and Pancreatic Lesions

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    机译 免疫组织化学在小儿非肿瘤性胃肠道，肝胆和胰腺病变中的当前应用综述
    摘要：Immunohistochemical (IHC) stains are widely used by pathologists for a variety of considerations in the diagnostic workup of pediatric nonneoplastic lesions in gastrointestinal (GI), hepatic, biliary, and pancreatic lesions. The pathologic changes cover a wide range and types of presentations, including inflammatory (bacterial and viral), metaplastic, posttransplant lymphoproliferative, autoimmune, metabolic, degenerative, developmental, and genetic conditions, among others. The everyday practical value of IHC stains covers primary identification, confirmation, differential, and/or exclusionary roles in the hands and eyes and minds of the practitioners. This article is intended to review and discuss the currently available IHC stains for a variety of pediatric GI, hepatobiliary, and pancreatic lesions as encountered in the day-to-day practice of pathologists and clinicians. It reflects the most recent methods and types of IHC stains with the stated aim of helping to provide a quick reference for diagnostic considerations and thereby facilitate the workup of a broad range of GI and related conditions in a pediatric population. The tables provide a handy reference on a wide range of IHC stains for commonly encountered lesions covering a variety of pediatric GI, hepatobiliary, and pancreatic conditions that are amenable to light microscopic diagnostic interpretation.
  • 8.

    【2hr】Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges

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    机译 高效液相色谱分析方法的验证及醋酸甲羟孕酮阴道内海绵的稳定性指示研究
    摘要：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.
  • 9.

    【2hr】Synthesis and Optical Properties of Pentamethine Cyanine Dyes With Carboxylic Acid Moieties

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    机译 具有羧酸部分的五甲胺花青染料的合成和光学性质
    摘要：Cyanine dyes possessing carboxylic acid groups have been used in many different fields of study. The acid groups can act as handles for bioconjugation or as metal chelators. Several pentamethine cyanine dyes with propionic acid handles were synthesized and their optical properties were studied to determine their usefulness as fluorescent probes. The optical properties studies performed include the absorbance and emission maxima values as well as the calculation of quantum yield and molecular brightness levels. Molecular models were also calculated to help analyze the dyes’ behavior and were compared with similar dyes with varying alkyl chain lengths replacing the acid moieties.
  • 10.

    【2hr】Quality by Design–Applied Liquid Chromatography-Tandem Mass Spectrometry Determination of Enzalutamide Anti-Prostate Cancer Therapy Drug in Spiked Plasma Samples

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    机译 通过设计应用液相色谱-串联质谱法测定加标血浆样品中恩扎鲁胺抗前列腺癌治疗药物的质量
    摘要：This research article presents the Quality by Design (QbD)–finalised conditions for a method that uses liquid chromatography-tandem mass spectrometry for the determination of concentration of enzalutamide (ENZ), an atypical anticancer drug, in a drug formulation and in spiked plasma samples. Critical process attributes (CPA) considered to be the influential parameters in separation, identification, and quantification processes by ultrahigh-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry (UHPLC-ESI-MS/MS) were organic content, buffer strength, pH modifier, flow rate, spray voltage, sheath gas, and auxiliary gas that alter critical analytical attributes, such as retention time (R1) and area (R2). These factors were evaluated first in a factorial design (Taguchi orthogonal array design) and then extensively in a central composite design (CCD) to zero-in on the mobile phase for the quantification of ENZ standard drug and along with its internal standard (ENZIS) in spiked plasma samples and in formulation. Pareto chart from initial factorial design (Taguchi orthogonal array design) model suggested which of the CPA factors should be given the weightage, that is, to be exhaustively analysed in the CCD and response surface analysis. The elaborated parameters proposed by World Health Organization were studied by method validation, ie, selectivity, linearity, accuracy, precision repeatability system-suitability tests, method robustness/ruggedness, sensitivity, and stability. The strategy followed gives an insight on the development of a robust QbD-compliant quantitative UHPLC-ESI-MS/MS method for ENZ drug containing plasma samples (spiked).
  • 11.

    【2hr】Comparison of 3 Derivatization Methods for the Analysis of Amphetamine-Related Drugs in Oral Fluid by Gas Chromatography-Mass Spectrometry

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    机译 气相色谱-质谱法分析口服液中苯丙胺类药物的三种衍生方法的比较
    摘要：The heptafluorobutyric anhydride (HFBA), pentafluoropropionic anhydride (PFPA), and trifluoroacetic anhydride (TFAA) are compared as derivatizing reagents to use as the optimal method for the analysis of 10 amphetamines and cathinones in oral fluid. The target compounds were amphetamine (AMP), methamphetamine (MA), 4-methylamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxy-N-ethylamphetamine (MDEA), cathinone (CAT), methcathinone, mephedrone, and ephedrine. Amphetamine-D5, MA-D5, MDA-D5, MDMA-D5, and MDEA-D5 use as internal standards (IS). The analytes and IS were extracted from 0.5 mL of oral fluid by ethyl acetate in the presence of NaOH (0.1 N) as the base and then the dried extracts were derivatized with HFBA, PFPA, or TFAA at 70°C for 30 minutes. The limits of quantification based on signal-to-noise ratios ≥10 were ranged between 2.5 and 10 ng/mL. The calibration graphs were linear in the range of 5 or 10 to 1000 ng/mL for all analytes. Based on sensitivity, the PFPA is proved to be the best for derivatization of the target compounds prior to gas chromatography-mass spectrometry analysis.
  • 12.

    【2hr】Insight into Biochemical Characterization of Plant Sesquiterpene Synthases

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    机译 深入了解植物倍半萜烯合酶的生化特性
    摘要：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.
  • 13.

    【2hr】Electrochemical Behavior and Voltammetric Determination of a Manganese(II) Complex at a Carbon Paste Electrode

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    机译 碳糊电极上锰（II）配合物的电化学行为和伏安法测定
    摘要：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.
  • 14.

    【2hr】Development and Validation of Stability-Indicating RP-HPLC Method for Simultaneous Determination of Metformin HCl and Glimepiride in Fixed-Dose Combination

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    机译 固定剂量组合同时测定盐酸二甲双胍和格列美脲的稳定性指示RP-HPLC方法的建立和验证
    摘要：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.
  • 15.

    【2hr】Quality Issues of Research Antibodies

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    机译 研究抗体的质量问题
    摘要：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.
  • 16.

    【2hr】Removal of 4-Nitrophenol from Water Using Ag–N–P-Tridoped TiO2 by Photocatalytic Oxidation Technique

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    机译 Ag-N-P-三掺杂TiO2光催化氧化去除水中的4-硝基苯酚
    摘要：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.
  • 17.

    【2hr】On the Conflicting Estimations of Pigment Site Energies in Photosynthetic Complexes: A Case Study of the CP47 Complex

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    机译 关于光合复合物中色素位点能量的有争议的估计：以CP47复合物为例
    摘要：We focus on problems with elucidation of site energies (E0n) 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 E0n 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 131-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.
  • 18.

    【2hr】Extraction of Honey Polyphenols: Method Development and Evidence of Cis Isomerization

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    机译 蜂蜜多酚的提取：方法开发和顺式异构化的证据
    摘要：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.
  • 19.

    【2hr】Stability-Indicating High-Performance Liquid Chromatography Assay for the Determination of Sulthiame in Pharmaceutical Dosage Forms

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    机译 稳定性指示高效液相色谱法测定药物剂型中的硫磺
    摘要：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.
  • 20.

    【2hr】Development of Hollow-Fiber Liquid-Phase Microextraction Method for Determination of Urinary trans,trans-Muconic Acid as a Biomarker of Benzene Exposure

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    机译 中空纤维液相微萃取法测定尿中反式，反式-葡糖酸作为苯的生物标志物的开发
    摘要：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.
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