超高效液相色谱-串联质谱法同时快速确证检测血浆和尿液中的42种精神药物及其代谢产物

针对公共卫生突发事件和临床毒物学检测实践中亟待解决的问题,建立了血浆和尿液中42种精神药物及其代谢产物的超高效液相色谱-串联质谱(UPLC-MS/MS)快速确证分析方法。样品经乙腈沉淀后,以乙酸铵和甲醇-乙腈(1:1, v/v)混合液作为流动相进行梯度洗脱,在Acquity UPLC BEH C18色谱柱上分离后用电喷雾串联质谱法检测,采用正、负离子快速切换多反应监测模式监测,基质标准同位素内标法定量。血浆样品中待测组分的加标回收率除了奋乃静、硫利哒嗪和氯丙嗪的分别为37.6%～57.5%, 36.3%～48.3%和52.4%～67.4%外,尿液样品中待测组分的加标回收率除了曲唑酮和地西泮的分别为100%～142%和108%～177%外,血浆和尿液中其余待测组分的加标回收率分别为60.2%～125%和64.5%～126%,相对标准偏差分别为0.8%～26%和2.6%～18%(n=6);除了巴比妥类药物的检出限为20～100 mg/L外,其余药物的检出限均为0.05～2.0 mg/L。该方法简单、快速、特异性强、灵敏度高。     

仪器定量分析中几个问题的探讨

详细介绍了分析方法的评价指标,包括检出限、测定限、灵敏度、精密度、准确度、动态范围和线性范围、抗干扰能力等,单因素优化方法与加标回收实验评定测定结果准确度的可靠性,并就分析工作中遇到的一些实际问题进行了讨论.     

载体的晶化对Ni/WO3-ZrO2催化剂结构及催化正庚烷异构化活性的影响

采用XRD、BET、IR、SEM、NH3-TPD方法对以无定形Zr(OH)4和已晶化的ZrO2为载体制备的Ni-WO3/ZrO2催化剂进行了表征,考察了载体晶化对催化剂结构、酸性及催化性能的影响。结果表明,载体晶化减弱了W与Zr间的相互作用,抑制了四方相ZrO2的生成,减少了催化剂上强酸中心的数目,从而降低了Pt-WO3/ZrO2催化剂上正庚烷异构化反应活性.     

铁磁性过渡离子掺杂对纤锌矿相硫化锌电子结构的影响

通过第一性原理计算,优化了铁磁性过渡离子掺杂的纤锌矿相硫化锌Fm0.125Zn0.875S(Fm=Fe、Co、Ni)的几何结构,计算了其电子结构,分析了其半金属性及其微观机制。结果表明:对不同的铁磁性杂质离子,Fm0.125Zn0.875S在费米面处的自旋极化率均为-100%,具有半金属性,是潜在的优质自旋注入材料。Fm0.125Zn0.875S具有较宽的自旋带隙,从而具有较高的居里温度和广泛的应用前景。Fe0.125Zn0.875S、Co0.125Zn0.875S和Ni0.125Zn0.875S的2×2×1超胞的磁矩分别为3.96μB、2.90μB和2.00μB,主要来自于铁磁性过渡离子Fe、Co和Ni离子。这3种离子的电子结构分别为eg2↑eg1↓t2g3↑,eg2↑eg2↓t2g3↑和eg2↑eg2↓t2g3↑t2g1↓。     

Structural Characterization and Retention Time Prediction for Components of Essential Oil of Meconopsis Integrifolia Flowers

A molecular structural characterization (MSC) method called reduced molecular electronegativity-distance vector (MEDVR) was used to describe the molecular structures of 55 components of meconopsis integrifolia flowers. By use of stepwise multiple regression (SMR) and partial least square (PLS) methods, a model with the correlation coefficient (R1) of 0.987 and the standard deviation (SD1) of 1.377 could be obtained. Then through multiple linear regression (MLR), another model with the correlation coefficient (R2) of 0.989 and standard deviation (SD2) of 1.395 could be constructed. Furthermore, in virtue of variable screening by the stepwise multiple regression technique (SMR), 8 vectors were selected to build up another model with its correlation coefficient (R3) and standard deviation (SD3) of 0.989 and 1.366, respectively. Then all the three models were evaluated by performing cross-validation with the leave-one-out (LOO) procedure, and the correlation coefficients (QCV) were 0.981, 0.976 and 0.979, respectively. The results show that the models constructed could provide estimation stability and favorable predictive ability.     

超高效液相色谱法测定纺织品中三氯生的含量

建立了快速准确测定纺织品中三氯生含量的高效液相色谱法,该方法以二氯甲烷为提取溶剂,超声提取了纺织品中的抗菌剂三氯生,提取液经浓缩吹干后用流动相定容,以甲醇-水(90∶10)为流动相,采用二极管阵列(PDA)检测器进行检测。该方法的线性范围为0.5~80 mg/L,检出限(S/N=3)为0.1 mg/L,回收率为95%~105%。     

配位化学的发展史

自从1893年瑞士化学家维尔纳创立配位化学已来,配位化学理论得到不断发展,逐渐完善。经过化学家们100多年的努力,由传统经典的配合物,发展到今天的配位超分子化合物,并显示出结构和功能上的优越特性,成为现代无机化学的一个发展方向。     

A Novel Inorganic-organic Hybrid Borate with Unique One-dimensional Infinite Aluminium-oxygen Chains

A novel inorganic-organic hybrid borate,[Al2(fum)(H3BO3)(OH) 4]n·n(H3BO3) (1,H2fum = fumaric acid) ,has been synthesized and characterized by single-crystal X-ray diffraction,FTIR and elemental analysis. Crystal data for compound 1: orthorhombic,space group Pnma,a = 14.108(3) ,b = 6.9412(14) ,c = 14.995(3) ,V = 1468.3(5) 3,Z = 4,Mr = 359.72,Dc = 1.627 g/cm3,μ = 0.254 mm-1,F(000) = 736,the final R = 0.0492 and wR = 0.1650 with I > 2σ(I) . In compound 1,each AlⅢ ion is coordinated by six oxygen atoms to adopt a distorted octahedral geometry. Both fumarate anion and the coordinated boric acid act as bidentate bridging ligands to link two neighboring AlⅢ centers simultaneously. Each AlⅢ ion is bridged by two μ2-hydroxyl ligands to construct an infinite wave-like [Al2(fum)(H3BO3)(OH) 4]n chain. These one-dimensional chains form hydrogen bonds with free boric acid molecules giving rise to a three-dimensional supramolecular network.     

几种纤锌矿相半金属铁磁体磁学性能的第一原理研究

通过基于密度泛函理论的第一原理计算,优化了纤锌矿结构的化合物TmZn15S16(Tm=V,Cr,Mn)的几何结构,并研究了它们的磁学性能.结果表明:TmZn15S16均为典型的半金属铁磁体,它们的超胞磁矩分别为3.0099μB,3.9977μB和5.0092μB;这些磁矩主要来源于被掺入的过渡元素;CrZn15S16的半金属特性比VZn15S16和MnZn15S16更稳定;这些半金属铁磁体的半金属带隙均比较宽,表明它们可能具有较高的居里温度;TmZn15S16中杂质过渡离子的电子结构分别为V:eg2↑t12g↑,Cr:eg2↑t22g↑和Mn:eg2↑t32g↑.     

Pt含量及活化温度对固体超强酸催化剂异构化性能的影响

本文制备了固体超强酸Pt- S2O82-/ZrO2-Al2O3催化剂,采用XRD、TPR、TG-DTA 、FT-IR等表征手段对催化剂进行了表征,并在高压微反－色谱联合装置上,考察了Pt质量分数和活化温度对催化剂正戊烷异构化性能的影响. 结果表明,Pt能使催化剂的还原温度降低;增强载体表面氢气的溢流效应,提高酸强度;Pt质量分数0.10%、活化温度300℃的催化剂异构化活性最高,在反应温度220℃、压力2.0MPa、氢烃摩尔比4:1、质量空速1.0h-1时,异戊烷产率达62.3%. 在100h内异戊烷收率可稳定在55%左右,选择性在98.0％以上.