Analysis of new psychoactive substances in human urine by ultra‐high performance supercritical fluid and liquid chromatography: Validation and comparison

New psychoactive substances represent serious social and health problem as tens of new compounds are detected in Europe annually. They often show structural proximity or even isomerism, which complicates their analysis. Two methods based on ultra high performance supercritical fluid chromatography and ultra high performance liquid chromatography with mass spectrometric detection were validated and compared. A simple dilute‐filter‐and‐shoot protocol utilizing propan‐2‐ol or methanol for supercritical fluid or liquid chromatography, respectively, was proposed to detect and quantify 15 cathinones and phenethylamines in human urine. Both methods offered fast separation (<3 min) and short total analysis time. Precision was well <15% with a few exceptions in liquid chromatography. Limits of detection in urine ranged from 0.01 to 2.3 ng/mL, except for cathinone (5 ng/mL) in supercritical fluid chromatography. Nevertheless, this technique distinguished all analytes including four pairs of isomers, while liquid chromatography was unable to resolve fluoromethcathinone regioisomers. Concerning matrix effects and recoveries, supercritical fluid chromatography produced more uniform results for different compounds and at different concentration levels. This work demonstrates the performance and reliability of supercritical fluid chromatography and corroborates its applicability as an alternative tool for analysis of new psychoactive substances in biological matrixes.     

高温作用后砂岩物理力学性质阈值温度的确定——基于机器学习算法

通过采用机器学习算法，提出了高温作用后砂岩物理力学性质变化的阈值温度的确定方法。基于Python语言，利用K-Means、SVM算法，实现了对样本数据的分类和聚类，确定了阈值温度区间，验证了二分类法的合理性和准确性.结果表明，砂岩样本的阈值温度区间为400~600 ℃，阈值温度上下砂岩的物理力学性质存在显著差异，体现为阈值温度区间以下的岩样物理力学性质较为分散，而阈值温度区间以上的岩样物理力学性质较为集中.     

高速电主轴热特性仿真与实验研究

对高速电主轴温度场分布随转速的变化规律进行了研究。通过在外壳上布置一定数量的温度传感器,对不同转速下的外壳温度进行实时测量,并将实验结果与ANSYS的模拟结果进行对比,验证了采用在电主轴外壳上布置多个测点测量与仿真相结合的方法来预测电主轴内部温度场分布的可行性;另外还分析了在不同转速下,高速电主轴关键部位的温升,仿真结果表明:主轴在6000~10000 r/min时,温升呈线性增加,在大于10000 r/min后,温升以指数规律增加。     

Fluorescence properties of riboflavin-functionalized mesoporous silica SBA-15 and riboflavin solutions in presence of different metal and organic cations

Riboflavin was covalently linked to mesoporous SBA-15 silica surface via grafting technique. Then fluorescence properties of the system obtained were analyzed in the presence of several metal and organic cations. Both quenching and strengthening of fluorescence as well as significant changes in the maximum fluorescence wavelength were observed. The results were compared with absorption and fluorescence data obtained for riboflavin water solutions.     

2008—2012年《中华实用儿科临床杂志》载文文献计量分析

目的:分析《中华实用儿科临床杂志》近5年发展情况,为提高该刊质量提供参考依据. 方法:通过"中国生物医学文献数据库"收集该刊2008—2012年的文献题录,采用文献计量学方法,对文献的时间分布、单位分布、作者分布、作者合作情况、单位合作情况、高频关键词、高频主题词等指标进行统计分析. 结果:2008—2012年《中华实用儿科临床杂志》共载文3 459篇,单篇论文的长度在逐年增长;涉及作者13 870位,每篇论文作者平均数量大于4,每篇论文的平均合作单位数量多于1.45,关键词和主题词符合本刊的主题.2008—2010年被引的文献为1 131条,占期间总文献量的62%.结论:2008—2012年发表的论文选择更具有针对性,向着更为合理性的方向发展,研究方法也多采用定量分析方法,并且论文形式多样,文献被引次数越来越多.     

Nonlinear frequency response analysis: a recent review and perspectives

The nonlinear frequency response analysis (NFRA) can be seen as an extension of electrochemical impedance spectroscopy. NFRA gives a full and detailed representation of the system response and can establish a connection between model parameters and the experimentally observed phenomena. In this article, different theoretical NFRA approaches and the most recent application examples are discussed. A simple electrochemical example is used to showcase the benefits and disadvantages of analyzing the system response by using different approaches. In addition, it was shown how to extract experimental harmonic values and analyze them.     

高静态动作压力下粉尘爆炸泄放标准的可靠性

粉尘爆炸泄放设计标准的可靠性对能否实现爆炸防护尤为关键.以中径70μm石松子粉尘为介质,采用20 L球形粉尘爆炸装置进行了4种泄放口径、静态动作压力在0.12~0.6 MPa的爆炸泄放实验,对比了实验值与NFPA 68和EN 14491计算值.结果表明,NFPA 68在预测高静态动作压力下的泄放面积时,随着泄放口径的增大,预测结果由保守变为危险,但预测结果精度较好且数值稳定;EN 14491在预测高静态动作压力下的泄放面积时非常保守,预测精度较差,数据不可靠.依据两种标准推荐的经验函数关系,分析了NFPA 68和EN 14491在预测高静态动作压力时产生这种差异的原因.     

宁波市公共自行车服务满意度评价模型构建研究

以宁波市公共自行车为例，将因子分析法与二项logistic法相结合，对采集的1 688份居民满意度有效问卷展开分析。利用因子分析法筛选出6个因子，利用二项logistic法剔除并筛选出5个有效因子构建公共自行车服务满意度评价模型，合理评估当前宁波市公共自行车服务满意度。同时，利用随机抽取并不参与建模的5%问卷样本对评价模型进行校验，以确保模型的准确性与合理性。该研究有助于合理评价当前宁波市居民对公共自行车的服务满意度，同时适用于对未来一段时间内公共自行车服务满意度的预测。     

Extraction of methyl xanthines and their UHPLC–DAD determination in consumable beverages used in Eastern province of Saudi Arabia

Coffee and tea are the most widely consumed beverages worldwide. However, the consumer may be unaware of the exact amount of methyl xanthine (MX, i.e. caffeine [C], theobromine [TB] and theophylline [TH]) consumed, as most of the products do not list the proper amounts. This may lead to serious risks including cardiovascular, kidney and stimulant effects. The aim of the study was to determine the MX amount in ready-to-use beverages (coffee and tea) collected from various outlets in the city of Al-Khobar, Saudi Arabia. Forty different samples of espresso, black coffee and red tea were collected. A fast, reliable and efficient UHPLC–DAD method was developed and validated for MX determination. Total lipids were extracted and fractionated in order to determine glycolipids, phospholipids and neutral lipids. The r² value for the method was 0.980–0.988 in a linearity range of 0.5–200 ppm. The range for MX (C [0.02–2.39 mg/ml], TB [0.00–0.10 mg/ml] and TH [0.00–0.004 mg/ml]) and total lipids was 1–5 g. The amount of glycolipids (3.1 g) was higher among the lipid fractions followed by phospholipids (1.8 g) and neutral lipids (0.25 g). In general, espresso beverages (20–30 ml) contained high amounts of MX whereas black coffee beverages contained high amount of lipids. Most of the beverages expressed C, TB, TH, lipids or their fractions; however, the product with high amounts of MX and lipids at the same time was espresso (brands Chemistry and Wogard). Although the MX and lipid levels in these beverages well below the allowed limits, care must still be taken, especially when using the beverages with high serving volumes (200–250 ml) or coffee prepared via the filter method i.e. black coffee, using a high temperature for a longer time.