顶空气相色谱法测定瑞替加滨原料药中残留溶剂

建立了测定瑞替加滨原料药中残留溶剂乙醇、正己烷、四氢呋喃、三乙胺的顶空气相色谱方法。采用氢火焰离子化检测器,以N,N-二甲基甲酰胺为样品溶剂,通过对色谱条件优化,建立了以DB-624为分析柱、110℃为平衡温度、15 min为平衡时间的残留溶剂测定方法。经方法学验证,上述4种溶剂的方法检出限依次为0.007 5%、0.000 48%、0.002 4%、0.01%;峰面积的相对标准偏差均小于2.1%;平均回收率为100%～102%;4种溶剂的线性系数均大于0.995。结果表明,该方法的检测灵敏度高、精密度好、准确度高、线性关系良好,能够满足对瑞替加滨质量的控制要求。将该方法应用于3批瑞替加滨原料药的残留溶剂检测,均只检出乙醇和正己烷,且乙醇和正己烷的最高残留量分别为0.149%和0.022%,均未超出限量规定。     

大学生学习成绩分析及相应的差异教学策略

以SPSS、Origin为主要数据分析工具,对某大学化工学院本科生期末考试成绩进行分析。对降序排列的平均学分绩点一元拟合曲线的残差进行了拟合,对其拟合函数进行求导,发现可以将样本按照20%、50%、30%的比例分为3个集团。通过层次聚类也得到类似的结果。不同集团的学生的学分获得率的组成、标准偏差分布明显不同。重要的专业基础课程在学生学习集团的形成中起到了重要的作用,基于统计结果,建议针对不同集团学生的学习特点应采取相应的差异化教学策略。     

Investigation on ion movement in the fringe-field switching mode depending on resistivity of alignment layer and dielectric anisotropic sign of liquid crystal

Adsorption and desorption of ions at interface between liquid crystal and alignment layer in liquid crystal displays play a crucial role in residual direct current voltage associated with image sticking. In this article, the dependency of such adsorption and desorption of ions on resistivity of alignment layer and sign of liquid crystal dielectric anisotropy in the fringe-field liquid crystal cell has been investigated. Our studies show that the time constant of ions during adsorption and desorption depends upon resistivity and dielectric constant of liquid crystal and alignment layer, and most strongly influenced by the resistivity of alignment layer such that the one with lower resistivity in two orders shows much faster adsorption and desorption at the interface than that of the one with higher resistivity.     

注塑制品残余应力的研究进展

由于实际工艺条件往往与理想值存在一定偏差,制品在成形后通常会存在一些难以避免的缺陷,而残余应力正是最为常见的一种。注塑制品的残余应力是在注塑成形过程中,外界约束去除后,仍存在于塑件内部的应力,在后期使用过程中容易引起塑件的翘曲、变形、乃至断裂破损,多数情况下对制品不利。因此,在塑料制品设计时应充分考虑到残余应力的影响。本文较为全面地介绍了注塑制品残余应力的产生、检测、减小残余应力的措施及残余应力的计算机模拟等内容。     

Orientation and conformation of two [6]carbohelicenes in stretched polystyrene and a thermoresponsive polyaspartate

Two functionalized [6]carbohelicenes, one of which was also available in its two enantiomeric pure forms, were oriented in stretched polystyrene in CDCl₃, and in a recently introduced chiral thermoresponsive lyotropic polyaspartate (poly(benzyl)_0.5(phenethyl)_0.5-L-aspartate) in C₂D₂Cl₄. From the resulting ¹H,¹³C residual dipolar couplings, the helical pitch of a methylated [6]carbohelicene was determined and found to be in agreement with theoretical predictions and existing crystal structures (d(C2,C2′) ≈ 4.3 Å). For a second [6]carbohelicene with para-methoxyphenyl substituents, a clear conformational preference of the substituents was observed. The orientational properties of the two helicene enantiomers in the chiral polyaspartate are very similar, but both drastically change around 306 K. We suggest this behavior is due to an unusual phase transition in the liquid crystal.     

化学发光酶免疫方法检测克伦特罗残留

建立了间接竞争化学发光酶免疫法(competitive indirect chemilumine scent enzyme immunoassy,ic-CLEIA)检测猪尿中残留克伦特罗(clenbuterol,CLB)的方法,并优化了竞争反应时间,Tween-20含量,PBS离子强度与pH4个参数。优化后的ic-CLEIA检出限可达0．01μg/L,检测范围为0．04～25．8μg/L,ED50为0．54μg/L;尿样检测的平均回收率为98％～120％,批内与批间相对标准偏差(variation of coefficent,CV)均小于10％。这些参数均优于目前广泛使用的ELISA方法,说明本CLEIA方法可替代ELISA法,用于实际尿样的检测。     

固相萃取高效液相色谱-质谱法测定动物组织中硝基呋喃代谢产物

研究了对动物组织中4种硝基呋喃类代谢产物AOZ、AMOZ、SEM和AHD的自动固相萃取HPLC-MS分析方法，分别以2-氯苯甲醛和2-硝基苯甲醛作为衍生化试剂，分别用AMOZ-d5、AOZ-d4作内标，用ENSPE柱进行提取，以乙腈-0．1％甲酸为流动相，采用梯度洗脱，可在15min内将4种代谢产物完全分离并进行测定。回收率为85％-90％；检出限可达0．5μg／kg。采用两种衍生化方法可获得较多的定性确证信息。采用本方法研究了硝基呋喃在鸡饲养过程中的残留规律。     

大口径毛细管气相色谱检查药物中残留溶剂的方法研究

 以药物合成中常用的 16种有机溶剂为研究对象 ,建立了用大口径毛细管柱检查残留有机溶剂的气相色谱法 ,并考察了不同极性的色谱柱及不同提取溶剂对分离与检测的影响。实验表明 ,根据原料药合成中可能存在的残留溶剂 ,选用适当的提取溶剂 ,采用大口径毛细管气相色谱法检查 ,可获得较满意的结果。     

Analysis of dimensionally stable copolyimide with a low‐level residual stress

Copolyimide thin film, which has low‐level stress and stress relaxation induced by water sorption, was characterized for potential applications as an encapsulant, a stress‐relief buffer, and in interlayer dielectrics. The polyimides examined were poly(p‐phenylene pyromellitimide) (PMDA‐PDA) and poly(p‐phenylene biphenyltetracarboximide) (BPDA‐PDA) as well as their random copolyimides with various compositions. These copolyimide films exhibited good combinations of physical and mechanical properties with low thermal expansion coefficients, residual stress, and moisture‐induced stress–relaxation behavior by appropriately selecting the ratios of the dianhydride component. For these polyimides, the residual stress increased in the range of −8.1–7.5 MPa, whereas stress relaxation induced by water uptake decreased in the range of 10.3–4.7 MPa with increasing BPDA contents, respectively. The major factor in determining the magnitude of the stress behavior induced by both the thermal mismatch and water uptake in films should be the morphological factors such as chain rigidity, chain orientation, crystallinity, and microvoids. Their morphological structures were examined by wide angle X‐ray diffraction and a prism coupler, and the thermal properties were measured using a dynamic mechanical thermal analyzer as well as thermomechanical analysis. Overall, the candidate for the low level stress buffer application from the PMDA/BPDA‐PDA copolyimide was the 30/70 (= PMDA/BPDA in molar ratio) copolyimide. This copolyimide showed no residual stress after curing at 400 °C and relatively insensitive stress relaxation to ambient humidity. © 2001 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 39: 796–810, 2001     

Phase Retrieval for Probability Distributions on Quantum Groups and Braided Groups

For nilpotent quantum groups [as introduced by Franz et al. ⁽⁷⁾], we show that (in sharp contrast to the classical case) the symmetrization of a probability distribution and the first moments of together determine uniquely the original distribution .