同位素内标-多反应监测同步在线质谱全扫描确证火锅料中罂粟壳成分

建立了高效液相色谱-三重四极杆线性离子阱质谱测定火锅料中吗啡、可待因、蒂巴因、罂粟碱、那可丁等5种生物碱残留的确证方法。样品采用稀盐酸加热提取,正己烷除脂,阳离子混合机理固相萃取柱净化,5%氨化乙酸乙酯-甲醇洗脱,PAK ST色谱柱分离,5 mmol/L乙酸铵甲醇溶液-10 mmol/L乙酸铵水溶液(pH 3.6)作为流动相洗脱,电喷雾正离子模式下多反应监测同步增强子离子在线全扫描(EPI)。在该实验条件下,5种生物碱的LOD在0.05~0.5 μg/kg之间,增强型子离子全扫描水平限和LOQ在0.2~2 μg/kg之间,方法回收率为64.2%~110.6%, RSD为4.2%~12.5%。阳性样品的定性确证需采用其子离子全扫描质谱图与标准图库中子离子质谱图检索匹配。经测定多种火锅料,表明本方法操作简单、测定结果准确,可用于火锅料中5种生物碱残留的阳性结果确证分析。     

Electrocatalytic Oxidation of Calcium Folinate on Carboxyl Graphene Modified CuxO/Cu Electrode

Carboxyl graphene modified Cu_xO/Cu electrode was fabricated. The bare copper electrode was firstly anodic polarized in 1.0 mol/L NaOH solution in order to get Cu_xO nanoparticles, then the carboxyl graphene (CG) was electrodeposited on the Cu_xO/Cu electrode by cyclic potential sweeping. The electrocatalytic oxidation behaviors of calcium folinate (CF) at the graphene modified Cu_xO/Cu electrode were investigated by cyclic voltammetry. A positive scan polarization reverse catalytic voltammetry was used to obtain the pure catalytic oxidation current. The graphene modified Cu_xO/Cu electrode was served as the electrochemical sensor of CF, a highly sensitivity of 22.0 μA·(μmol/μL)^-1cm^-2 was achieved, and the current response was linear with increasing CF concentration in the range of 2.0×10^-7 mol/L to 2.0×10^-5 mol/L, which crossed three orders of magnitude, and the detection limit was found 7.6×10^-8 mol/L (S/N=3). In addition, the proposed sensor was successfully applied in determination of CF in drug sample.     

Disposable Screen‐Printed Edge Band Ultramicroelectrodes for the Determination of Trace Amounts of Nitrite Ion

The application of linear scan voltammetry for sensitive determination of nitrite by using a disposable screen‐printed edge band carbon ultramicroelectrode (designated as SPUME) was reported in this study. The measurement with the SPUME can be performed in solutions of low ionic strength, e.g., natural waters, because the ohmic loses are negligible. The limiting oxidation current of nitrite showed a wide linear range up to 3 mM at the SPUME. A relative standard deviation of 2.46% (n=5) for analyzing 5 μM nitrite indicated a detection limit (S/N=3) of 0.38 μM. Real sample analysis of mineral and ground water samples as well as bratwurst food product showed satisfactory results. Since the SPUME is low cost and easy for mass production, the disposable nature further offers to application in diverse field of electroanalytical chemistry.     

Differential scanning calorimetry study on thermal behaviors of freeze‐dried poly(L‐lactide) from dilute solutions

Glass transition, cold crystallization, and melting of freeze‐dried poly(L‐lactide) (PLLA) prepared from dilute 1,4‐dioxane solutions were investigated by differential scanning calorimetry (DSC). Conventional DSC measurements of heating scans revealed that freeze‐dried PLLA prepared from a 0.07 wt % solution undergoes a two‐step cold crystallization (or reorganization) with a lower exotherm appearing at about 78 °C and with a higher broad exotherm between 110–155 °C. The peak temperature of the former exotherm is about 50 K lower than that observed for a reference bulk sample. Step‐scan mode DSC, which provides information essentially equivalent to that obtained from the temperature‐modulated DSC, revealed that the glass‐transition temperature is about 6 K lower than that of the reference bulk. These findings suggest enhanced chain mobility for freeze‐dried PLLA. Freeze‐dried PLLA that crystallized at 80 °C for 40 min was revealed to contain a rather large amount of rigid amorphous material (42%). © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 115–124, 2005     

光针扫描法检测光滑表面粗糙度

提出了一种用于光滑表面粗糙度测量的方法，利用两个标准参考面和两个偏振片实现对表面粗糙度的测量，通过两1／4波片克服光路可逆性的缺陷，给出了测量系统光路图，导出了该方法工作原理的数学表达式，并对该方法产生的测量不确定度进行了理论计算与计算机仿真，最后通过对一标准粗糙度样块进行测量，证明了该方案的可行性。结果表明实测值与样块厂家提供的标称值相符，并可实现0．2nm的测量精度。     

Distributions of the Numbers of Failures and Successes in a Waiting Time Problem

Abstract. In this article we consider infinite sequences of Bernoulli trials and study the exact and asymptotic distribution of the number of failures and the number of successes observed before the r-th appearance of a pair of successes separated by a pre-specified number of failures. Several formulae are provided for the probability mass function, probability generating function and moments of the distribution along with some asymptotic results and a Poisson limit theorem. A number of interesting applications in various areas of applied science are also discussed.     

团簇WOS3Cu3I(2-MePy)3激发态非线性光学性质

用Z扫描方法测量了团簇WOS3Cu3I(2 MePy) 3对 5 32nm、8ns激光脉冲的非线性光学响应曲线。以速率方程为基础对实验结果进行拟合 ,理论计算和实验结果符合得很好。应用激发态折射理论研究了非线性折射率系数的符号变化和折射度比值Kr 的关系 ,Kr>1时非线性折射率系数为正 ,Kr<1时折射率系数为负。     

一种新的电子束扫描电流产生方法

 在工业辐照电子直线加速器中,电流发生器是电子束扫描设备中的重要部分,可控式电流反馈-电流镜产生扫描电流是一种新方法,其电流波形可被扫描均匀度指标修正,不仅可以得到良好的电子束扫描均匀度,而且还可以提高均匀扫描的速度。     

半花菁LB膜的三阶非线性特性

本文利用Z扫描测量技术首次对半花菁LB膜的三阶非线性光学特性进行了研究.实验结果表明,LB多层膜中的半花菁分子具有较高的三阶非线性折射率n²=2.0×10^-8(esu),这主要是半花菁分子中π电子体系的贡献,并且由于532nm在其Q吸收带内,引起三阶非线性的共振增强效应,实验数据与理论拟合结果符合得很好.半花菁LB膜的三阶非线性的响应时间在30ns以内.     

宣德官窑青花瓷的面扫描分析

用SRXRF对宣德时期官窑青花瓷片上的瓷彩进行面扫描分析,结果表明各元素分析线的峰面积有着不同的分布模式。根据与颜色浓淡、瓷彩上黄斑的耦合关系可以将K,Cr,Mn,Fe,Co,Ni,Cu,Zn,Hg,Rb,Sr,Y和Zr等13个元素分为3组。它可作为各个朝代青花瓷“指纹元素”的选择依据,并提出了研究瓷彩中黄斑的形成机制的新思路。