液相色谱串联质谱法测定水果中复硝酚钠残留量

以甲醇提取样品,采用超高效液相色谱串联质谱法(UPLC–MS/MS)测定水果中复硝酚钠的残留量。以甲醇–10 mmol/L乙酸铵水溶液(体积比为60∶40)为流动相,质谱采用电喷雾负离子MRM检测模式。对硝基苯酚钠和5-硝基愈创木酚钠的线性范围为0.05~2.00 mg/L,检出限为0.01 mg/kg,邻硝基苯酚钠的线性范围为2.5~100.0 mg/L,检出限为0.5 mg/kg,线性相关系数均大于0.995。实际样品中对硝基苯酚钠、邻硝基苯酚钠和5-硝基愈创木酚钠的加标回收率分别为83.0%~93.4%,81.0%~87.4%,83.0%~91.8%,测定结果的相对标准偏差小于7%(n=6)。该法操作简单、快捷,精密度、准确度高,适用于水果中复硝酚钠的残留分析。     

反胶束固定化醇脱氢酶的制备及应用研究

研究十六烷基三甲基溴化铵(CTAB)-辛烷-己醇反胶束体系固定化醇脱氢酶(ADH)的制备及应用。考察了含水量、CTAB和己醇用量对于ADH固定化的影响。对游离酶和固定化酶的催化动力学性质研究表明:酶促反应的最适pH值分别为8.2和8.8,最适温度分别为31℃和20℃,米氏常数分别为12mmol/L和7mmol/L。30℃时,游离酶存放150min后失活90%,固定化酶失活50%,表明反胶束固定化ADH有较好的热稳定性。应用此体系测定了试样中乙醇的含量。     

高效液相色谱-串联质谱法同时测定茶汤中7种苯甲酰脲类农药残留

建立了高效液相色谱-串联质谱(HPLC-MS/MS)法,结合溶剂提取和固相富集技术同时测定茶汤中氟啶脲、除虫脲、啶蜱脲、氟虫脲、氟铃脲、伏虫隆和杀铃脲7种苯甲酰农药残留的方法。研究了提取溶剂的种类、用量和提取时间,以及固相富集小柱的固定相和流动相对7种苯甲酰脲类农药的提取率、分离度、灵敏度和重现性等的影响。结果表明,在最佳条件下,7种苯甲酰脲类农药在6.5min内被完全分离。7种苯甲酰脲类农药残留的检测限(DL)和定量限(QL)分别为0.08~1.00ng/mL和0.09~3.02ng/mL,加标回收率为90%~105%,相对标准偏差(RSD)小于7%(n=6)。利用所建立的方法成功测定了不同茶汤中上述7种苯甲酰脲类农药残留。该方法具有耗时短、灵敏度高、稳定性好等优点,有助于茶叶安全饮用的准确评价。     

Synthesis of Nitrogen Doped Multilayered Graphene Flakes: Selective Non‐enzymatic Electrochemical Determination of Dopamine and Uric Acid in presence of Ascorbic Acid.

Nitrogen doped multilayered graphene (NDMLG) is synthesized by annealing the black fluffy mass obtained by decomposing the complex prepared from Zn(OAc)₂, diethanolamine and triethanolamine. The NDMLG has been characterized by HRTEM, FESEM, XRD, XPS, Raman spectroscopy, BET which indicate formation of nitrogen doped multilayer graphene flakes with high surface area. NDMLG shows better electrochemical oxidation property towards Dopamine, Uric acid and Ascorbic acid. The linear response ranges for determination of DA, UA and AA are 0.5–150 µM, 3–60 µM and 80–2000 µM respectively and the detection limits (S/N=3) are 15 nM, 15 nM, 580 nM, respectively in the mixture.     

Discrimination Between 8‐Oxo‐2′‐Deoxyguanosine and 2′‐Deoxyguanosine in DNA by the Single Nucleotide Primer Extension Reaction with Adap Triphosphate

The adenosine derivative of 2‐oxo‐1,3‐diazaphenoxazine (Adap) exhibits a superb ability to recognize and form base pairs with 8‐oxo‐2′‐deoxyguanosine (8‐oxo‐dG) in duplex DNA. In this study, the triphosphate of Adap (dAdapTP) was synthesized and tested for single nucleotide incorporation into primer strands using the Klenow Fragment. The efficiency of dAdapTP incorporation into 8‐oxo‐dG‐containing templates was more than 36‐fold higher than with dG‐containing templates, and provides better discrimination than does the incorporation of natural 2′‐deoxyadenosine triphosphate (dATP). The selective incorporation of dAdapTP into 8‐oxo‐dG templates was therefore applied to the detection of 8‐oxo‐dG in human telomeric DNA sequences extracted from H₂O₂‐treated HeLa cells. The enzymatic incorporation of dAdapTP into 8‐oxo‐dG‐containing templates may provide a novel basis for sequencing oxidative DNA damage in the genome.     

An improved scheme for determining heat transfer correlations from heat exchanger regression models with three unknowns

A nonlinear regression scheme for determining heat transfer correlations from overall heat exchanger measurements is presented. The proposed scheme is valid for any two-fluid heat exchanger data where only one fluid's thermal resistance varies. The resulting regression model has three unknowns; two are associated with the variable resistance, and the third is the sum of all other resistances. The model can be analyzed only by using nonlinear regression because it cannot be transformed into linear form. Unlike existing approximate methods of analysis (known as modified Wilson plots), the proposed scheme is guaranteed to converge if a solution exists. The scheme was successfully tested by analyzing data collected on a tube-fin heat exchanger with continuous plain fins.     

卫星惯性/星光组合自主定姿方法研究

利用星敏感器测量所得的恒星星光方向信息,采用六状态变量推广卡尔曼滤波,得到卫星姿态误差和陀螺漂移误差信息并进行相应的修正。仿真结果表明,这种方法修正效果良好,采用中等精度陀螺组件就可以实现高精度定姿;仿真结果还验证了陀螺随机误差、星敏感器测量噪声和滤波周期等因素对定姿精度的影响。     

基于多视场星敏感器的姿态确定方法

星敏感器是目前航天器姿态测量精度最高的器件,与传统的单视场星敏感器相比,多视场星敏感器可以实现三轴同样高精度的姿态测量,提高姿态测量精度。针对单视场星敏感器姿态确定问题,推导了以最小代价函数为指标的QUEST姿态确定算法。对于多视场星敏感器,通过坐标变换方法将多个视场的导航星矢量转换到同一视场中,再利用QUEST算法得到航天器姿态。最后仿真结果表明,坐标变换后进行姿态确定得到的姿态数据与单个视场所得的姿态数据相同,验证了方法的正确性。     

基于粒子滤波的微小卫星姿态确定算法

为了提高非线性卫星姿态控制系统的滤波性能,在建立了采用磁强计及太阳敏感器的卫星姿态模型的基础上尝试了新兴的粒子滤波(PF)算法对卫星系统进行姿态估计,进而对采用矢量观测的三轴稳定卫星的姿态确定问题进行了滤波算法的实时仿真,并将四元数转换成旋转矢量引入了粒子滤波算法,最后给出了卫星模型在不同粒子数目下的滤波性能比较,并在系统初始误差较大的情况下将粒子滤波算法与EKF滤波算法进行了滤波性能的对照。仿真结果表明,粒子滤波算法对粒子数目具有明显的依赖性,但是当粒子达到一定的数目时,粒子滤波的精度以及滤波稳定性都可以得到保证,尤其是在系统初始误差较大的情况下粒子滤波算法更显示了其优于EKF算法的滤波性能。     

???????????????????????????????

应用动态应变测试方法对悬挂式残膜回收机悬挂架进行实地动应力测 试，通过数据处理及其分析，得到悬挂架在工作条件下的应力状态，以及不同工作状态下各 构件的应力情况，并对悬挂架进行了疲劳强度分析，为进一步改进设计提供必要的理论依据.