气相色谱-负化学源质谱联用法测定菊酯类农药

通过固相萃取-气相色谱-负化学离子源质谱技术建立了11种拟除虫菊酯类农药残留的检测方法，并应用于茶叶农残检测。样品经乙酸乙酯提取后，用串联的活性炭和中性氧化铝固相萃取柱选择性地富集茶叶中待测组分，再由气相色谱-负化学离子源质谱分时段选择离子监测技术进行测定。方法简单快速，一次进样就能得到11种菊酯残留结果；准确度和精密度高，在0．016μg／kg、0．032μg／kg和0．064μg／kg3个添加水平下的回收率在70％～110％之间，CV≤7．4％；选择性好，消除了色素和其它杂质干扰；灵敏度高，检出限低，除了氯菊酯为10μg／kg外，其它菊酯检出限都在μg/∥kg级，七氟菊酯则达到了0．02μg／kg。     

Kinetics of glass transition,crystallization and soft magnetic properties of the Fe76.5Nb3B20Cu0.5 glassy alloys

Journal of Thermal Analysis and Calorimetry - Differential scanning calorimetry was used to investigate the non-isothermal crystallization kinetics of the Fe76.5Nb3B20Cu0.5 glassy alloys. The...     

气相色谱-负化学离子源质谱法检测食品中苯醚甲环唑的残留量

建立了一种用于各种食品中苯醚甲环唑残留量的气相色谱-负化学离子源质谱(GC-MS/NCI)检测方法。用乙酸乙酯对各类样品中的苯醚甲环唑进行提取,固相萃取(SPE)净化后由GC-MS/NCI在选择离子监测模式下进行测定。方法的准确度和精密度高,多数样品在0.01,0.04,0.10 mg/kg三个添加水平下苯醚甲环唑的回收率处于70%和120%之间,相对标准偏差（RSD）不大于9.5%。方法在0.02～1.00 mg/L范围内有良好的线性关系,且灵敏度高,最低检测限达到0.0005 mg/kg;选择性好,抗干扰能力强,能消除复杂基质带来的干扰,适合各种食品中苯醚甲环唑残留量的确证分析。     

高效液相色谱-串联质谱法测定蜂蜜中残留的19种喹诺酮类药物

建立了高效液相色谱-电喷雾串联质谱联用测定蜂蜜中恩诺沙星、环丙沙星、诺氟沙星、氧氟沙星、双氟沙星、恶喹酸、氟甲喹、沙拉沙星、司帕沙星、丹诺沙星、氟罗沙星、马波沙星、伊诺沙星、奥比沙星、吡哌酸、培氟沙星、洛美沙星、西诺沙星和萘啶酸等19种喹诺酮类药物残留的方法。比较酸性溶液阳离子固相萃取(PCX柱)、近中性缓冲溶液反相固相萃取（HLB柱）和碱性溶液阴离子固相萃取(PAX柱)3种不同提取净化方法的提取效果,最终选择使用碱性溶液溶解蜂蜜样品,强阴离子固相萃取柱一步富集净化。以甲醇和0.1%甲酸溶液作为流动相,C18作为分析色谱柱,采用梯度洗脱方式进行液相色谱分离,选择离子反应监测模式检测19种喹诺酮类药物,内标方法定量。在1～100 μg/L范围内,19种喹诺酮类药物的线性相关系数均大于0.991。通过实际样品的添加回收试验,方法的定量限（S/N=10）为1.0 μg/kg,3个添加水平的回收率为71%～118%,相对标准偏差为4.2%～6.7%。     

Analysis of stability for a discrete ratio-dependent predator-prey system

The paper investigated the dynamical behaviors of a two-species discrete ratio-dependent predator-prey system. The local stability of the equilibria is obtained by using the linearization method. Further, a new sufficient condition on the global asymptotic stability of the positive equilibrium is established by using an iteration scheme and the comparison principle of difference equations.     

Adaptive Modified Function Projective Lag Synchronization for Two Different Chaotic Systems with Stochastic Unknown Parameters

In this paper, we investigate the modified function projective lag synchronization for two different stochastic chaotic systems using adaptive control method. We design an adaptive controller to make the mean square of synchronization error convergence to an arbitrarily small bound around zero depending on the controller feedback gain according to the Lyapunov stability theory. One example is presented to demonstrate the effectiveness of the proposed controller.

     

两种离子化技术气相色谱-质谱法测定橄榄油中甾醇烯类物质的比较

分别采用电子轰击(EI)和正化学电离(PCI)两种离子源技术建立了气相色谱-质谱联用法(GC-MS)同时测定橄榄油中3,5-菜甾二烯、3,5,22-豆甾三烯和3,5-豆甾二烯3种甾醇烯含量的方法,并对这两种方法进行了比较。样品经石油醚溶解,硅胶柱净化后,分别采用GC-EI/MS和GC-PCI/MS分时段选择离子监测模式进行测定,以3,5-胆甾二烯为内标进行定量。结果表明,两种方法的线性、准确度、精密度、灵敏度均较好。3,5-菜甾二烯、3,5,22-豆甾三烯和3,5-豆甾二烯分别在0.024~0.48、0.02~0.50和0.03~0.75 mg/L浓度范围内线性关系良好(r>0.999)。在3个加标水平下,GC-EI/MS和GC-PCI/MS的平均回收率分别为88.7%~99.5%、87.1%~109.2%,两种检测方法的相对标准偏差(RSD,n=6)均不超过8.3%。定量限(S/N=10)分别为0.03 mg/kg(EI),0.03~0.10 mg/kg(PCI)。通过对两种方法的比较研究发现,EI能提供更多碎片离子和结构信息,而PCI中则主要为准分子离子及反应气加合离子。应用于样品中甾醇烯的测定时,PCI的选择性和抗干扰能力明显优于EI。两种方法可相互补充和替代应用于日常检测中。     

两种离子源技术气相色谱-质谱法检测茶叶中酰胺类除草剂的残留量

采用电子轰击(EI)和负化学(NCI)离子源两种离子源技术气相色谱-质谱联用法(GC     

Calorimetric study on Ge<Subscript>23</Subscript>Se<Subscript>67</Subscript>Sb<Subscript>10</Subscript>–0.5CsCl glass

The mechanical behavior of Ge₂₃Se₆₇Sb₁₀ glass can be improved by adding CsCl facilitating the nano-crystaline formation. Understanding the crystallization mechanism of chalcogenide glass can help in directing the subsequent annealing processing and tuning the microstructure and physical properties. In this work, 99.5Ge₂₃Se₆₇Sb₁₀–0.5CsCl glass was prepared and its transformation kinetics was investigated under non-isothermal conditions with heating rate up to 400 K min^?1. Using Vogel–Fulcher–Tammann equation, the ideal glass transition temperature was determined as T _0g = 434.1 K. Using the classical JMA theory, the average activation energy and average growth exponent were determined as 135.0 and 2.4 kJ mol^?1, while using the model considering impingements (MCI), the two parameters were determined as 120.9 and 3.2 kJ mol^?1, respectively. Compared to JMA theory, the MCI model can fit the transition curves better, and it shows that the growth mode of the present glass is between two-dimension and three-dimension. By comparing with the result of Ge₂₃Se₆₇Sb₁₀ glass, it is found that addition of CsCl can reduce the growth dimension and activation energy during crystallization.     

激光核聚变装置中基于像传递的激光自动准直技术研究

基于像传递的激光自动准直技术是提高准直准确度、增加稳定性的好方法。本文在理论上用两快速傅里叶变换（ＦＦＴ）分析了准直中基于像传递的近远场信号对图像处理影响。在光束近无场像面上引入十字叉丝并以“神光”装置的某一级空间滤波器为例,计算出光束直径一定时合适的十字叉丝尺寸;最后通过实验确定了基于像传递的自动直技术的具体实现系统。