表面解吸常压化学电离质谱快速分析六味地黄丸

采用新型表面解吸常压化学电离(Surface Desorption Atmospheric Pressure Chemical Ionization, SDAPCI)质谱法, 在敞开环境下, 对潮湿的空气进行电晕放电产生试剂离子, 进而在六味地黄丸表面发生解吸电离过程, 在无需复杂预处理的前提下对六味地黄丸中的待测物进行离子化, 从而获得了六味地黄丸在正负离子模式下的化学指纹图谱, 并利用主成分分析法对质谱指纹数据进行处理, 可对6个厂家生产的多个批次产品进行较好的区分. 结果表明, SDAPCI-MS技术能够快速测定六味地黄丸的剂型和生产厂家信息, 并能够对目标组分做多级串联质谱鉴定, 发现痕量目标组分. 研究方法可望应用于中成药药品生产质量控制和成品检测等领域.     

Neutral desorption extractive electrospray ionization mass spectrometry for fast screening sunscreen agents in cream cosmetic products

High throughput analysis of sunscreen agents present in cream cosmetic has been demonstrated, typically 2 samples per minute, using neutral desorption extractive electrospray ionization mass spectrometry (ND-EESI-MS) without sample pretreatment. For the targeted compounds such as 4-Aminobenzoic acid and oxybenzone, ND-EESI-MS method provided linear signal responses in the range of 1-100 ppb. Limits of detection (LOD) of the method were estimated at sub-ppb levels for the analytes tested. Reasonable relative standard deviation (RSD = 8.4-16.0%) was obtained as a result of 10 independent measurements for commercial cosmetics samples spiked with each individual sunscreen agents at 1-10 ppb. Acceptable recoveries were achieved in the range of 87-116% for direct analysis of commercial cream cosmetic samples. The experimental data demonstrate that ND-EESI-MS is a useful tool for high throughput screening of sunscreen agents in highly viscous cream cosmetic products, with the capability to obtain quantitative information of the analytes.     

MgB2颗粒超导体临界电流的温度特性研究

通过制备MgB2/MgO超导复合材料,获得了典型的MgB2弱连接颗粒超导体,并测量了该样品在不同温度下的Ⅰ-Ⅴ特性曲线.在Ⅰ-Ⅴ曲线中,我们发现:当电流超过临界电流时,电压随着电流先是缓慢的增长,在电流升到一定值时,电压有一个很陡的突变.我们对这一变化进行了研究,认为这是由于MgO杂质使MgB2的晶界效应增强所引起的.该样品的临界电流和温度的关系满足:jc(T)∝(1-T/Tc)1/3,利用三维Josephson结网络系统的渗流模型进行计算发现,当颗粒超导系统处于非均匀状态时,临界电流和温度满足关系式jc(T)∝(1-T/Tc)4/3,这一结果和我们的实验符合的非常好.     

石墨炉原子吸收光谱法测定麦麸颗粒中镉

为消除石墨炉原子吸收光谱法测定麦麸中镉时基体产生的背景干扰,在消解液中加入镉标准溶液配制基体匹配工作曲线进行测定,对灰化温度、原子化温度及基体改进剂等条件进行优化,确定最佳分析方法。结果表明：在选定条件下镉在0.0~3.0 μg/L范围内工作曲线相关系数为0.9991,检出限为0.027 μg/L,定量限为0.091 μg/L,加标回收率为89.50%~104.12%,精密度为1.64%~4.30%,质控物质测定结果准确。该方法操作简便,快速准确,精密度良好,适用于麦麸中镉元素的测定。     

Coupling corona discharge for ambient extractive ionization mass spectrometry

Unlike the extractive electrospray ionization (EESI) technique described elsewhere, a corona discharge instead of electrospray ionization has been utilized to charge a neutral solvent spray under ambient conditions for the generation of highly charged microdroplets, which impact a neutral sample plume for the extractive ionization of the analytes in raw samples without any sample pretreatment. Using the positive ion mode, molecular radical cations were easily generated for the detection of non-polar compounds (e.g., benzene, cyclohexane, etc.), while protonated molecular ions of polar compounds (e.g., acetonitrile, acetic ether) were readily produced for the detection. By dispensing the matrix in a relatively large space, this method tolerates highly complex matrices. For a given sample such as lily fragrances, more compounds were detected by the method established here than the EESI technique. An acceptable relative standard deviation (RSD 8.9%, n = 11) was obtained for the direct measurement of explosives (10 ppb) in waste water samples. The experimental data demonstrate that this method could simultaneously detect both polar and non-polar analytes with high sensitivity, showing promising applications for the rapid detection of a wide variety of compounds present in complex matrices.     

Study of adsorption performance and adsorption mechanism for U(VI) ion on modified polyacrylonitrile fibers

Journal of Radioanalytical and Nuclear Chemistry - The modified polyacrylonitrile fibers (ACPAN fibers) was synthesized by oximation reaction and alkaline hydrolysis. ACPAN fibers was characterized...     

Recyclable Polyurea-Urethane Thermosets with De-Crosslinking Capability in Acetic Acid

Chinese Journal of Polymer Science - Covalent crosslinking points within thermosets generally result in excellent mechanical properties and solvent resistance yet lead to limited degradability and...