Development, validation and transfer of a hydrophilic interaction liquid chromatography/tandem mass spectrometric method for the analysis of the tobacco-specific nitrosamine metabolite NNAL in human plasma at low picogram per milliliter concentrations

A highly sensitive bioanalytical method based on a simple liquid/liquid extraction and hydrophilic interaction liquid chromatography with tandem mass spectrometry (HILIC/MS/MS) analysis has been developed, validated and transferred for the determination of 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL), a tobacco-specific nitrosamine metabolite. Deuterated NNAL (NNAL-d(4)) was synthesized and used as the internal standard. This method can be used for the analysis of free and total NNAL (free NNAL plus NNAL-gluc) in K(3)-EDTA human plasma. Free NNAL and NNAL-d(4) are extracted from human plasma by liquid/liquid extraction. To analyze for total NNAL and the internal standard, a separate aliquot of the K(3)-EDTA human plasma is treated with beta-glucuronidase to deconjugate the NNAL-gluc; the total NNAL and internal standard are then extracted using liquid/liquid extraction. After drying down under nitrogen, the residue is reconstituted with acetonitrile and analyzed using positive ion electrospray and HILIC/MS/MS at a flow rate of 1.0 mL/min. The chromatographic run time is 1.0 min per injection, with retention time for both NNAL and NNAL-d(4) of 0.75 min with a capacity factor (k') of 2. The standard curve range for this assay is from 5.00-1000 pg/mL for both free and total NNAL, using a total plasma sample volume of 1.0 mL. The interday precision and accuracy of the quality control (QC) samples demonstrated <7.6% relative standard deviation (RSD) and <3.3% relative error (RE) for free NNAL. For total NNAL, the interday precision and accuracy of the QC samples demonstrated <11.7% RSD and <2.8% RE. Optimization of enzyme hydrolysis of NNAL-gluc is discussed in detail. The overall recoveries for free and total NNAL and IS were 68.2 and 71.5% (free) and 70.7 and 65.5% (total). No adverse matrix effects were noticed for this assay.     

KINETICS OF SUSPENDED EMULSION POLYMERIZATION OF METHYL METHACRYLATE

The kinetics of suspended emulsion polymerization of methyl methacrylate (MMA), in which water acted as the dispersed phase and the mixture of MMA and cyclohexane as the continuous phase, was investigated. It showed that the initial polymerization rate (Rp0) and steady-state polymerization rate (Rp) were proportional to the mass ratio between water and oil phase, and increased as the polymerization temperature, the potassium persulphate concentration ([I]) and the Tween20 emulsifier concentration ([S]) increased. The relationships between the polymerization rate and [I] and [S] were obtained as follows: Rp0 ∝ [I]0.73[S]0.32 and Rp ∝ [I]0.71[S]0.23. The above exponents were close to those obtained from normal MMA emulsion polymerization. It also showed that the average molecular weight of the resulting poly(methyl methacrylate) decreased as the polymerization temperature, [I] and [S] increased. Thus, MMA suspended emulsion polymerization could be considered as a combination of many miniature emulsion polymerizations proceeding in water drops and obeyed the classical kinetics of MMA emulsion polymerization.     

贫困大学生就业对策研究

随着高等教育快速发展,高校毕业生就业形势越来越严峻。本文从家庭经济贫困对大学生的专业学习、能力培养、就业信息获取、就业观念等造成负面效应入手,探讨就业对策,从而帮助贫困生实现充分就业。     

DCS的接地分析

文章对分散型计算机控制系统几种不同的接地方式作了详细分析，并对在系统接地装置安装过程中出现的技术问题及注意事项提出了相应处理措施及说明。     

粉煤灰烧结坯体性能试验研究

研究粉煤灰粘土坯体的成型条件、烧结温度、最大粉煤灰掺量3个方面对坯体性能的影响，得到粉煤灰砖生产的最优方案，为粉煤灰砖的实际生产提供理论依据。     

集聚纺集聚区须条等截面部分的力学分析

通过对集聚区内须条的集聚过程分析，建立须条的受力模型，发现须条在集聚过程中会产生附加捻度，并且对影响须条附加捻度的各种因素：异型管开槽长度、负压大小、须条和网格套圈间的摩擦因数以及异型管的曲率半径进行了分析。设计相关实验对集聚区内须条的力学模型进行了验证。结果表明所建立的集聚区内须条的力学模型是正确的。     

钪对铝锂合金再结晶温度的影响

通过硬度测量和微观金相观察,研究了钪对铝锂合金再结晶过程的影响.结果表明,向铝锂合金加入微量的钪,可以在合金中形成尺寸细小、密集度高而且弥散分布的Al3Sc和Al3(Scx,Zr1-x)相粒子,能有效阻碍位错的移动和亚晶界的迁移与合并,稳定亚晶结构,对晶界有很强的钉扎作用,从而抑制了再结晶晶粒的形核与长大,提高了铝锂合金的再结晶温度.     

从藏书排架谈种次号的确定方法

针对种次号排架存在的弊端，提出了若干改进方法，在一定程度上解决了内容特征基本相同的图书或适宜集中排架的图书不能集中的问题，便于读者在查找图书过程中的挑选与比较。     

拟南芥抗盐单基因突变体的诱导与筛选

用Co60-γ射线辐照野生型拟南芥种子，将诱变处理后的M一代种子温室种植，收获的M2代种子用于抗盐突变体的筛选，将在200mmol／L盐胁迫条件下筛选出的352株幼苗根仍表现向地性生长或真叶不变为褐色的植株作为可能的突变体，再将这些M2代可能的突变体移苗种植至基质中并收获M3代种子，经对M3代的抗盐性状继续进行检测，最终获得4株100％表现抗盐性状的突变体。     

光子晶体用PS/Ti(OBu)4复合乳胶粒的制备

将乳液聚合形成的聚苯乙烯乳胶粒子在苯／无水乙醇／钛酸丁酯的混合液中溶胀，使钛酸丁酯在溶胀吸附过程中进入乳胶粒内部，以构制复合乳胶粒子，并用红外光谱、透射电镜和差热分析等方法对复合乳胶粒子的组成、形貌、热稳定性和热转变进行了研究。结果表明，在苯／无水乙醇／钛酸丁酯混合介质中，聚苯乙烯乳胶粒并不溶解，但可以溶胀，并吸入钛酸丁酯，经水解后，形成聚苯乙烯／二氧化钛乳胶粒，二氧化钛最高含量可达10％左右。