Dynamic ultrasound-assisted extraction of polyphenols in tobacco

A novel extraction method, namely dynamic ultrasound-assisted extraction, is investigated. This technique is efficient with respect to both time and solvent consumption because it utilizes ultrasonic energy in dynamic mode during extraction. Polyphenols (chlorogenic acid, esculetin, rutin, scopoletin, and quercitrin) are extracted from a tobacco (Nicotina tobaccum L.) sample for 10 min with 6 mL of solvent. Fresh solvent is continuously pumped through the sample, with which the analytes can be rapidly extracted, and the possibility of degradation efficiently avoided. Methanol involving 0.5% w/v ascorbic acid was used as extraction solvent; optimal flow rate and extraction time were investigated. The extract was cleaned up by C18 disposable cartridge. The spiked and nonspiked tobacco samples were used for the evaluation of the proposed method. Recoveries obtained were varied from 96 to 108% and RSDs from 2.0 to 4.6%. This extraction technique was revealed to recover larger amounts of polyphenols from tobacco, compared to the static ultrasound-assisted extraction method.     

含铈多元氧化物的活性结构及在丙烯氨氧化中的作用

本文利用流化床反应器研究了多元复合氧化物PMo_(12)Bi_3Fe_(8-x)Ce_xK_(0.1)O_y(x=0-8)中稀土元素铈对丙烯氨氧化的催化作用,并用x-射线衍射、红外光谱、扫描电镜和热重技术表征了催化剂的结构,发现x=2-3时,丙烯腈的收率最高。催化剂中存在Fe_2(MoO_4)_3,Ce_2(MoO_4)_3、α-Bi_2O_3、3MoO_3。这三种物相的互相溶解和凝结形成固溶体和准均相,使活源。份在各物相表面或界面上均匀分布,由此产生的各活性组份的协调作用是催化活性的主要来性组铈能抑制MoO_3升华,稳定活性相结构。     

A stereoselective synthesis of squalamine

Squalamine (1) was synthesized stereoselectively in 14 steps and 19% overall yield from 3-keto-5-chenodeoxycholanate (2) by using a modified Sharpless asymmetric dihydroxylation as the key step.     

Determination of sulfur dioxide in vitriol plant wastewater by using a polyNiMe4TAA electrochemically modified Pt microelectrode

A Pt microelectrode modified with nickel(II) polytetramethyldibenzo[b,i]tetraaza[14]annulene was prepared by electropolymerization of nickel(II) tetramethyldibenzo[b,i]tetraaza[14]annulene monomers and applied to determine sulfur dioxide in vitriol plant wastewater. For determination of SO2 with this electrochemically modified Pt microelectrode, the linear range was from 9.6 x 10(-6) to 2.4 x 10(-4) mol L-1, the sensitivity was 1.8 x 10(-4) A L mol-1, the detection limit was calculated to be 4.8 x 10(-6) mol L-1 (S/N = 3), the response time was less than 20 s and the relative standard deviation was found to be 2.1% on analyzing 4.8 x 10(-5) mol L-1 SO2 solution repeatedly (n = 7). These results demonstrated good accuracy compared with those obtained by the conventional iodimetric method.     

The uranium-Xylidyl Blue I complex and its application in linear sweep polarography

The linear sweep polarographic wave of the uranium-Xylidyl Blue I complex in ethylenediamine-1,10-phenanthroline-hydrochloric acid medium has been studied. The complex, corresponding to UO(2)(XBI)(2-)(2) with log beta' = 9.09 (by polarography), 8.81 (by spectrophotometry), is strongly adsorbed on the surface of the mercury electrode. The polarographic wave is attributed to the reduction of Xylidyl Blue I in the complex. The method is very sensitive with a detection limit of 3 x 10(-8)M. The wave height is proportional to the concentration of uranium over the range 8 x 10(-8)-7 x 10(-6)M. Solvent extraction is used to separate possible interferences. The recommended procedure has been applied to the determination of trace amounts of uranium in ores.     

Preparation and application of selenite ion selective electrode

A new selenite ion selective electrode using 4,6-dibromopiaselenole as active material, PVC as membrane matrix and dibutyl phthalate as plasticizer has been developed. An analytically useful potential change occurs from about 10(-6)-10(-1)M Se(IV), and the slope of the linear portion is -23.6 mV/10-fold change in Se(IV) concentration at a temperature of 21 degrees . The electrode shows fairly good selectivity for selenite ion over other anions and has been used for the successful determination of total selenium in human hair.     

磺化聚苯硫醚铑配合物催化剂初探

苯硫醚具有与三苯基磷相似的配位化学性能,膦类配体具有比苯硫醚强的络合能力,但毒性较大,热稳定性和抗氧稳定性不如苯硫醚类配体。能否以含有机硫的配体替代膦类配体,这是开发新型催化剂的一个值得探索的方向。聚苯硫醚经发烟硫酸磺化后,可制得水溶性的磺化聚苯硫醚。经XPS测定,磺化度为     

钇与2-(4′-氯-2′-膦酰基一苯偶氮)-7-(2′,6′-二溴-4′-氯-一苯偶氮)-1,8-二羟基-3,6-萘二磺酸配位反应动力学研究和机理探讨

用停流分光光度法获得反应的经验速率方程为R=k[y(H_2O~n)~(3+)]·[H_6R]·[H~+]~(-1)。参考Eigen-Tamm机理和测得的动力学参数,拟出了反应的可能机理。     

A nonlinear regression model applied to kinetic studies of ester hydrolysis with a surface acoustic wave sensor

A non-linear regression model was derived for the simultaneous determination of the rate constant in alkaline hydrolysis of esters and the initial concentration of esters based on the linear relationship between the frequency response of the surface acoustic wave sensor system and the conductivity of the solution. The model was tested theoretically and experimentally with the methyl-, ethyl-, and n-propyl-acetate systems. The corresponding rate constants estimated at 25 degrees C are 0.147, 0.103 and 0.0671 respectively.     

光化学-荧光分析法研究——Ⅲ.片剂及注射液中安定的测定

本文提出了测定安定的光化学—荧光分析新方法。安定在含有十二烷基硫酸钠的稀硫酸介质中,经紫外光照射后,产物能发射荧光(=368nm,=476nm)。安定浓度在0～2.5μg/ml范围内,荧光强度与浓度成良好的线性关系。方法的相对标准偏差为1.5％,检出限为0.044μg/ml,可用于片剂及注射液中安定含量的测定。