Kinetics of polyesterification: Adipic acid with ethylene glycol, 1,4-butanediol,and 1,6-hexanediol

Polyesterifications of adipic acid with ethylene glycol, 1,4-butanediol, and 1,6-hexanediol in the absence and presence of the foreign acid (p-toluene sulfonic acid) as catalyst were carried out under constant reaction temperatures of 140–180°C (rather than at constant oil-bath temperatures) and at ratios of diol to diacid of 0.9867–3.5880. The experimental data fit the rate equations proposed by Chen and Wu: d(RCOOR′)/dt = k_ae^αp(RCOOH)²(R′OH) – k_h(H₂O)(RCOOR′) and d(RCOOR′)/dt = k_ac(AH)e^αp(RCOOH)(RO′H) – k_h(H₂O)(RCOOR′) for self-catalyzed and acid-catalyzed reactions, respectively; the data did not fit the other equations appearing in the literature. Here p is the conversion of acid, and α is the constant related to dielectric constants. The reaction rate constants and activation energies for self-catalyzed and acid-catalyzed reactions are calculated. The activation energy is found to decrease with chain length of the alkyl group of the diol. This result is consistent with that observed by Brauman and Blair using ion cyclotron resonance spectroscopy for the variation of acidity of alcohols with chain length of the alkyl group.     

Simultaneous Determination of Six Immunosuppressants in Human Whole Blood by HPLC-MS/MS Using a Modified QuEChERS Method

A high-performance liquid chromatography-tandem mass spectrometry method was established for the simultaneous determination of mycophenolic acid, mycophenolate mofetil, tacrolimus, rapamycin, everolimus and pimecrolimus in human whole blood by optimizing the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) preparation method. Whole blood was extracted into ethyl acetate, salted out with anhydrous magnesium sulfate, and purified with ethylenediamine-N-propyl silane adsorbent. The supernatant was evaporated under nitrogen until dry and finally reconstituted in methanol. Chromatographic separation was performed on an Agilent Poroshell 120 EC-C18 column in methanol (mobile phase A)-water (optimized for 0.1% acetic acid and 10 mM ammonium acetate, mobile phase B) at a 0.3 mL·min⁻¹ flow rate. Electrospray ionization and positive ion multiple reaction monitoring were used for detection. The time for of analysis was 13 min. The calibration curves range of tacrolimus, rapamycin, everolimus and pimecrolimus were in the range of 1–100 ng·mL⁻¹, mycophenolate mofetil in the range of 0.1–10 ng·mL⁻¹ and mycophenolic acid at 10–1000 ng·mL⁻¹. All correlation coefficients were >0.993. The coefficients of variation (CV, %) for inter-day and intra-day precision were less than 10%, while the spiked recoveries were in the range of 92.1% to 116%. Our method was rapid, sensitive, specific, and reproducible for the simultaneous determination of six immunosuppressants in human whole blood. Importantly, our approach can be used to monitor drug concentrations in the blood to facilitate disease treatment.     

香花石形态所反映的一种可能的孪晶结构

香花石是我国发现的第一个新矿物,它的形态非常复杂.本文基于香花石形态上出现了左形与右形相聚的现象,对香花石形态进行了重新思考,认为同一单形的左形与右形不能相聚形成单晶体,只能形成孪晶,因此,对原香花石晶体图进行了一些修正,认为原香花石晶体图可能是一个孪晶图.这对深入认识晶体形态及晶体对称理论、澄清长期以来人们并没有足够重视的一些基本概念有重要意义.     

ISOVALEROYL OXOKADSURANE,A NOVEL DIBENZOCYCLOOCTADIENE LIGNAN POSSESSING A SPIROBENZOPURANOID SKELETON

Isovaleroyl oxokadsurane, a novel dibenzocyclooctadiene lignan pos-sessing a spirobenzofuranoid skeleton was isolated from the stems of Kadsura coccinea.Its structure and relative configuration were determined by X-ray diffraction analysis.     

高效液相色谱法同时测定生物质乳酸发酵液中有机酸及糖类化合物

建立了高效液相色谱(HPLC)同时测定生物质乳酸发酵液中有机酸及糖类的分析方法。使用Bio-Rad Aminex HPX-87H色谱柱,以5 mmol/L的H2SO4为流动相,在柱温55 ℃,流速0.6 mL/min条件下,采用示差折光检测器进行检测。结果表明,该方法可在17 min内实现发酵液中各种有机酸和糖类化合物等的完全分离与定量,6种有机酸和3种糖类化合物在0.15～5.19 g/L范围内的线性关系良好,回归方程的线性相关系数在0.9998以上。将该法用于米根霉发酵液的检测,两个水平的加标回收率为96.91%～103.11%,相对标准偏差(n=6)为0.81%～4.61%。该法适用于微生物发酵液中多种有机酸和糖类的快速、高效分离和定量测定。     

FNR-Ⅰ核磁共振波谱仪

基于自旋回波的原理研制成功了一台专用于分析磁性材料的核磁共振波谱仪。其工作频率为25-80MHz;输出功率10W,可用它在77-300°k范围测量铁磁材料的共振谱线,增强因数和自旋-自旋弛豫时间T₂;它也可用于测量非磁性固体的宽核磁共振谱线。     

BRST cohomology and highest weight vectors. I

We initiate a program to study certain recent problems in non-compact coset CFT by the BRST approach. We derive a reduction formula for the BRST cohomology by making use of a twisting by highest weight modules. As illustrations, we apply the formula to the bosonic string model and a rank one non-compact coset model [DPL]. Our formula provides a completely new approach to non-compact coset construction.Partially supported by NSF Grant DMS-8703581