国产高分辨飞行时间质谱仪在药物分子结构鉴定中的应用

为了考察自主研发的API-TOF MS 10000电喷雾高分辨飞行时间质谱仪（ESI-TOF MS）对离子准确质量数测定的准确性及其在新药研发中的应用前景,采用该仪器对新药研发中涉及的291个天然产物及合成物进行质谱分析。以三氟乙酸钠为内标物进行仪器质量轴校准,将测试得到的目标离子准确质量数与理论准确质量数对比,计算两者的相对误差。结果表明：248个样品的分子质量测试结果与预期一致;对其中202个样品进行高分辨质谱测试,所得实验值与理论准确质量数之间的相对误差均小于5×10^-6;与预期不一致的实验结果提示样品的结构解析有误,并得到了其他波谱数据的验证。采用API-TOF MS 10000和美国AB Sciex公司的QSIAR Elite型Q/TOF MS对抗癌药物马来酸阿法替尼和降糖药利格列汀杂质进行质谱分析。结果表明,自主研发的API-TOF MS 10000与国际同类仪器对药物分子准确质量数的测试结果无明显差异,可以提供化合物准确的分子质量和分子式信息,是新药研发中药物分子结构解析的有力工具。     

Development of a practical foolproof system using ultrasonic local positioning

The objective of this research is to develop a prototype for practical foolproof system which can be used in manual assembly processes. For this purpose, a high-performance and low-cost ultrasonic system is proposed to measure 3D positions of an indoor mobile object. Composed of an ultrasonic sender and a receiver, the system employs ultrasonic time-of-flight (TOF) and trilateration to estimate the positions of the object with an accuracy of few centimeters. To calculate three TOFs, ultrasonic signals are processed full-digitally with a low-cost FPGA, which provides high design flexibility keeping both high performance and low noise. Proposed system is autonomous, so there is no need of an external PC and the system development cost becomes low. As an improved thresholding method to calculate the TOFs, this paper proposes a debounce module, designed in the FPGA, to remove the pulse noises generated during the thresholding. The resulting time delay from the debounce is compensated by a microprocessor for calculating actual TOFs. Lastly, the positions of the mobile object are calculated from the TOFs values by trilateration in the microprocessor. In order to remove measurement noises, both moving average filters and Kalman filters are adopted in calculating the TOFs and positions.     

Decomposition of NO over Cu-AITS-1 zeolites

H-AITS-1 zeolite with Si/Ti = 50 and Si/Al = 50 was employed in preparing catalyst samples by ion-exchange and impregnation with a copper nitrate solution to obtain 0.24–1.15 wt.% and 1.5, 2 and 2.5 wt.% Cu loading, respectively. The catalytic properties for the NO decomposition were compared with that of Cu-ZSM-5 (Si/Al = 25 with 2 wt.% Cu loading) and similarity was found between the AITS-1 based samples and Cu-ZSM-5. Due to the higher acidity, the activity at 500°C per total copper atoms (an apparent turnover frequency, TOF) was significantly higher over Cu based AITS-1 samples being 2–3 × 10⁻³ s⁻¹ as compared to 1 × 10⁻³ s⁻¹ measured on Cu-ZSM-5. For the ion-exchanged Cu-AITS-1 there was an increase in TOF with increasing copper content, whereas on the impregnated samples a decrease in TOF was found. On all catalysts there was a maximum in the NO conversion at 500–550°C. The amount of NO per copper atom measured by temperature programmed desorption (TPD) was about the same as that on Cu-ZSM-5 and the features of the TPD were also similar. At the first contact of the catalyst at 500°C with the 2 vol% NO/Ar gas a transient N₂O formation and a considerable delay in the O₂ formation was observed. This could, however, be reproduced only on fresh catalyst, while all further transients showed different but reproducible features using the same sample.     

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry of Vernonia galamensis oil

Matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) mass spectrometry (MS) has been used to identify eight triacylglycerols (TAG) in Vernonia galamensis oil (VO). The TAG include trivernolin, divernoloylstearoylglycerol, divernoloyloleoylglycerol, vernoloyllinoleoylstearoylglycerol, vernoloyllinoleoyloleoylglycerol, and vernoloyldilinoleoylglycerol. Samples for the MALDI/TOF/MS analysis were prepared with alpha-cyano-4-hydroxycinnamic acid (matrix) in an acetonitrile/tetrahydrofuran solvent system. A mol ratio of matrix/VO (44:1) gave reproducible composite spectra, resulting in resolutions greater than 8,000 and signal-to-noise ratios of above 1000 for the most abundant molecular species. 1,3-Dioleoyl-2-stearoylglycerol and 1,2-dioleoyl-3-palmitoylglycerol were used as calibration standards.     

Chemical Profiling Using Uplc Q‐Tof/Ms and Antioxidant Activities of Fortunella Fruits

The fruits of Fortunella Swingle are widely consumed as fresh fruits and traditional medicine in China. China is the origin center and has the largest cultivated area of the genus Fortunella. In this study, the chemical compositions of ethanol extracts of the major Fortunella cultivated types including Fortunella japonica Swingle, Fortunella margarita Swingle, Fortunella crassifolia Swingle 1 (Lanshang) and Fortunella crassifolia Swingle 2 (Liuyang) were determined using ultra performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry (UPLC Q‐TOF/MS) method, and their antioxidant activities were evaluated. 12 compounds were identified and 5 compounds were tentatively characterized. The results showed that the chemical compositions of the ethanol extracts of 4 Fortunella cultivated types were largely the same. 3′, 5′‐di‐C‐glucopyranosylphloretin was the predominant flavonoid in Fortunella fruits, and Fortunella margarita Swingle had higher contents of flavonoids than other species. In addition, the data demonstrated high antioxidant activities of Fortunella fruits. The developed method could be available to rapidly analyze the chemical compounds in Fortunella fruits and its products. This study will provide information for further quality assessment and utilization of Fortunella resources.     

BESⅡ顶点探测器径迹组合触发判选系统

在ＢＥＳⅡ中顶点探测器代替了ＢＥＳ的中心漂移,建立了相应的触发判选子系统。介绍了ＢＥＳⅡ顶点探测器触发判选子系统的原理,构成,逻辑设计和结果。该系统是北京谱仪触发判选系统升级改进的主要项目之一。     

快中子探测器的效率刻度

本文叙述了用n-p散射方法刻度快中子探测器效率的基本原理、实验方法和测量结果。400 keV氘束轰击T-Ti靶,由T(d,n)~He反应得到15.2 MeV的中子,散射体是一个圆柱塑料闪烁体(φ2.2×3cm),飞行距离2m,时间分辨率约1.5ns,效率测量的能区范围为1—14MeV,对多次散射和几何条件作了修正,总的误差约2%。     

透射型定时探测器

本文介绍了由微道板构成的透射型定时探测器,得到的飞行时间系统的时间分辨为280ps。并对进一步改善时间特性作了讨论。     

BESⅢ TOF子触发系统击中信息多通道串行同步传输方法

为了获得抗干扰、抗辐射能力强的远距离数据传输,在第三代北京谱仪BESⅢ工程的TOF前端电子学与TOF子触发系统之间采用了光纤传输方案。同时为了节省空间,在发送端对并行数据进行并串转换然后传送串行数据。然而接收端串并恢复的过程中会存在每次上电同步后转换延时不确定性的现象,从而导致了串并转换恢复数据/时钟的摇摆问题。在探讨现象本质的基础上,结合FIFO的同步功能,提出了可以广泛适用的系统同步法以及一种适用于目前数据传输方案的简便同步方法,成功地实现了多通道并串/串并转换数据的串行同步传输。