夏季东亚副热带反气旋进退活动的非线性机理讨论

采用三维强迫耗散非线性动力学模式,结合夏季东亚副热带地区实际的环流结构和天气特征,对东亚上空副热带反气旋的活动进行了研究和探讨,导出了系统稳定性的位涡拟能判据并据此进行了分析和讨论·所得判据可为分析和预报夏季东亚上空副热带高压的进退变化及相应的东亚天气提供参考依据·     

基于属性识别准则大学生思想品德量化的数学模型

依据一定的社会评价标准,建立大学生思想品德评价的指标体系,利用现代数学方法——属性识别理论和层次分析方法,建立定量研究模型.     

Development of Improved High-Performance Liquid Chromatography Method for the Determination of Residual Caprylic Acid in Formulations of Human Immunoglobulins

Quality control of human immunoglobulin formulations produced by caprylic acid precipitation necessitates a simple, rapid, and accurate method for determination of residual caprylic acid. A high-performance liquid chromatography method for that purpose was developed and validated. The method involves depletion of immunoglobulins, the major interfering components that produce high background noise, by precipitation with acetonitrile (1:1, v/v). Chromatographic analysis of caprylic acid, preserved in supernatant with no loss, was performed using a reverse-phase C18 column (2.1 × 150 mm, 3 μm) as a stationary phase and water with 0.05% TFA–acetonitrile (50:50, v/v) as a mobile phase at a flow rate of 0.2 mL/min and run time of 10 min. The developed method was successfully validated according to the ICH guidelines. The validation parameters confirmed that method was linear, accurate, precise, specific, and able to provide excellent separation of peaks corresponding to caprylic acid and the fraction of remaining immunoglobulins. Furthermore, a 2⁴⁻¹ fractional factorial design was applied in order to test the robustness of developed method. As such, the method is highly suitable for the quantification of residual caprylic acid in formulations of human immunoglobulins for therapeutic use, as demonstrated on samples produced by fractionation of convalescent anti-SARS-CoV-2 human plasma at a laboratory scale. The obtained results confirmed that the method is convenient for routine quality control.     

Free mycophenolic acid determination in human plasma ultrafiltrate by a validated liquid chromatography–tandem mass spectrometry method

The aim of this study was to develop and validate fully the liquid chromatography–tandem mass spectrometry method for free mycophenolic acid (MPA) concentration measurements in plasma ultrafiltrate that will be reliable and simple in preparation with deuterated MPA (MPA‐d3) chosen as an internal standard. The chromatographic separation was made with Zorbax Eclipse XDB‐C18 column (4.6 × 150 mm) using a gradient of two solutions as a mobile phase: (A) water and (B) methanol, each containing 0.1% formic acid and 2.5 mm ammonium acetate. Satisfactory repeatability of retention times was achieved with average values of 7.54 ± 0.20 min and 7.50 ± 0.19 min for MPA and MPA‐d3, respectively. The method was selective, with no carry‐over or matrix effect observed. The analytical range was proven for MPA ultrafiltrate concentrations of 1–500 ng/mL. The accuracy and precision fell within the acceptance criteria for intraday (accuracy: 100.63–110.46%, imprecision: 6.23–7.76%), as well as interday assay (accuracy: 98.81–110.63%; imprecision: 5.36–10.22%). The method was used for free MPA determination in plasma samples from patients treated with mycophenolate mofetil. To the best of our knowledge this is the first liquid chromatography–tandem mass spectrometry method for free MPA monitoring using MPA‐d3 that allows to measure plasma ultrafiltrate concentrations as low as 1 ng/mL.     

Novel rapid liquid chromatography tandem masspectrometry method for vemurafenib and metabolites in human plasma,including metabolite concentrations at steady state

A novel, rapid and sensitive liquid chromatography tandem–mass spectrometry method for quantification of vemurafenib in human plasma, that also for the first time allows for metabolite semi‐quantification, was developed and validated to support clinical trials and therapeutic drug monitoring. Vemurafenib was analysed by precipitation with methanol followed by a 1.9 min isocratic liquid chromatography tandem masspectrometry analysis using an Acquity BEH C₁₈ column with methanol and formic acid using isotope labelled internal standards. Analytes were detected in multireaction monitoring mode on a Xevo TQ. Semi‐quantification of vemurafenib metabolites was performed using the same analytical system and sample preparation with gradient elution. The vemurafenib method was successfully validated in the range 0.5–100 μg/mL according to international guidelines. The metabolite method was partially validated owing to the lack of commercially available reference materials. For the first time concentration levels at steady state for melanoma patients treated with vemurafenib is presented. The low abundance of vemurafenib metabolites suggests that they lack clinical significance. Copyright © 2016 John Wiley & Sons, Ltd.     

Simultaneous analysis of 35 specific antihypertensive adulterants in dietary supplements using LC/MS/MS

A sensitive and specific LC/MS/MS method was developed for the simultaneous analysis of 35 compounds used for treating hypertension as adulterants in dietary supplements. The method was validated for specificity, linearity, accuracy, precision, limit of detection, limit of quantitation, stability and recovery. The limit of detection and limit of quantitation ranged from 0.20 to 20.0 and 0.50 to 60.0 ng/g, respectively. The linearity was good (r ² > 0.999), with intra‐ and interday precision levels of 0.43–7.87% and 0.65–9.95% and the intra‐ and interday accuracies of 84.36–115.82% and 83.78–118.69%, respectively. The stability (relative standard deviation) was <14.75%. The mean recovery was 80.81–117.86% (relative standard deviation <10.00%). Ninety‐seven commercial dietary supplements available in South Korea were analyzed. While none contained detectable amounts of the 35 antihypertensive compounds, the developed LC/MS/MS procedure can be used for routine analysis to monitor illegal adulteration in various forms of dietary supplements.     

Locomotion of vehicles on hinged road mats

In this paper, the hinged road-mat construction is modeled as a cable structure, and based on the equivalent cable theory the sinkage of the roadway is evaluated. Neglecting details of the interaction between tires and road mats, works caused by the traction, resistance, and drawbar pulling are defined to build a new work criterion to evaluate the mobility of vehicles on the hinged road mats. Mobility diagrams, related to coefficient of adhesion, terrain deformation, beam width, and fastening force, are developed to evaluate the locomotion of vehicles and further guide the design of hinged road mats. The presented method compares well with the field terramechanical experiments of the hinged road mats, thus verifying the validity of equivalent cable modeling and work criterion for hinged road mats.     

LR12‐peptide quantitation in whole blood by RP‐HPLC and intrinsic fluorescence detection: Validation and pharmacokinetic study

A simple, sensitive, selective and robust HPLC method based on intrinsic fluorescence detection was developed for the quantitation of a dodecapeptide (designated as LR12), inhibitor of Triggering Receptor Expressed on Myeloid cells‐1, in rat whole blood. Sample treatment was optimized using protein precipitation and solid‐phase extraction. Chromatographic separation was carried out in a gradient mode using a core–shell C₁₈ column (150 × 4.6 mm, 3.6 μm) with mobile phases of acetonitrile and water containing trifluoroacetic acid at 1.0 mL/min. The method was validated using methodology described by the US Food and Drug Administration guidelines for bioanalytical methods. Linearity was demonstrated within the 50–500 ng/mL range and the lower limit of quantitation was 50 ng/mL. Finally, a preliminary pharmacokinetic study after intraperitoneal injection of LR12 in rats was conducted to evaluate both LR12 monomer and its corresponding disulfide dimer, the main product of degradation. Beyond the fact that this paper describes the first fully validated method for LR12 analysis in blood samples, the approach followed here to optimize pre‐analytical steps could be beneficial to develop HPLC and/or MS methods for other pharmaceutical peptides.     

A GENERALIZED MODELING FOR CEMENT-BASED MATERIALS UNDER LARGE RANGE OF COMPRESSION STATE

The aim of this study is to describe the main behavior of cement-based materials under large compression state based on the recent experimental research. In this paper, the strainstress relations are firstly analyzed and confining pressure state is regarded as low/medium/high state. A generalized cup modeling is introduced by a coupled deviatoric shearing, pore collapse and damage mechanism within thermodynamic framework. A series of numerical simulations are performed for the considered cement paste and concrete. Comparisons between numerical predictions and experimental results show that the proposed model is able to describe the main features of mechanical behavior under large range of compression state.     

Validation and clinical application of an LC‐ESI‐MS/MS method for simultaneous determination of tolmetin and MED5, the metabolites of amtolmetin guacil in human plasma

A highly sensitive, rapid assay method has been developed and validated for the simultaneous estimation of tolmetin (TMT) and MED5 in human plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive‐ion mode. A simple solid‐phase extraction process was used to extract TMT and MED5 along with mycophenolic acid (internal standard, IS) from human plasma. Chromatographic separation was achieved with 0.2% formic acid–acetonitrile (25:75, v/v) at a flow rate of 0.50 mL/min on an X‐Terra RP₁₈ column with a total run time of 2.5 min. The MS/MS ion transitions monitored were 258.1 → 119.0 for TMT, 315.1 → 119.0 for MED5 and 321.2 → 207.0 for IS. Method validation and clinical sample analysis were performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 20 ng/mL and the linearity was observed from 20 to 2000 ng/mL, for both the anlaytes. The intra‐day and inter‐day precisions were in the range 3.27–4.50 and 5.32–8.18%, respectively for TMT and 4.27–5.68 and 5.32–8.85%, respectively for MED5. This novel method has been applied to a clinical pharmacokinetic study. Copyright © 2010 John Wiley & Sons, Ltd.