新显色剂1－（对－偶氮苯）－3－（2－噻唑）－三氮烯与锌显色反应的研究及应用

本文研究了新显色剂１－（对－偶氮苯）－３－（２－噻唑）－三氮烯在非离子表面活性剂ＴｒｉｔｏｎＸ－１００存在下，与锌（Ⅱ）显色反应的适宜条件。结果表明，在ｐＨ１３．０～１４．０范围内，锌（Ⅱ）与题示试剂形成１：３的稳定粉红色配合物，其最大吸收波长为５４５ｎｍ，试剂的最大吸收波长为４６３ｎｍ。配合物表现摩尔吸光系数在５４５ｎｍ处为９．６×１０￣４Ｌ·ｍｏｌ￣（－１）＊ｃｍ￣（－１）；０～２４μｇ／２５ｍＬＺｎ符合比耳定律。该试剂对锌的选择性良好。方法用于铝合金中锌的直接测定，结果令人满意。     

A Polarographic Study of ϵ-Caprolactam Complexes of Uranium and Tellurium

The polarographic behaviour of uranium and tellurium has been studied in the presence of increasing concentration of complex forming agent viz. ?-caprolactam at pH 4.4 for U(VI) and at pH 10.0 for Te(IV) at μ=0.1 M KNO₃. In both cases the waves have been found to be diffusion controlled and irreversible. The values of kinetic parameters (σπ_a and K°_f,h) have been calculated as a function of the ligand concentration. Method is suitable for the quantitative determination of these metals individually and simultaneously with the effect of diverse ions.     

Spectrophotometric studies and analytical application of Ce(III) chelates with 1-(2-pyridylazo)-2-naphthol (PAN)

A sensitive procedure for spectrophotometric determination of cerium(III) has been developed. AtpH 10.2 cerium reacts with 1-(2-pyridylazo)-2-naphthol in 40% ethanol to form a red complex which has an absorption maximum at 545 nm. The molar absorptivity at 545 is 3.95·10³ mol^–1. Maximum stability of the complex was attained in pure ethanol. The stoichiometries and structures of the chelates were studied applying conductometric titration, visible spectrophotometry and IR spectrophotometry. The IR spectra revealed that coordination takes place through the N=N, C-OH and pyridyl group.

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Spektrophotometrische Untersuchungen und analytische Anwendung von Ce(III)-Chelaten mit 1-(2-Pyridylazo)-2-naphthol (PAN)

Zusammenfassung Es wurde eine empfindliche Methode zur spektrophotometrischen Bestimmung von Cer(III) entwickelt. Bei einempH von 10,2 reagiert Cer mit 1-(2-Pyridylazo)-2-naphthol in 40% Ethanol unter Bildung eines roten Komplexes mit einem Absorptionsmaximum bei 545 nm (=3 950). Der Komplex besitzt in reinem Ethanol ein Maximum an Stabilität. Die Stöchiometrien und Strukturen der gebildeten 1:1- und 1:2-Chelate wurden mittels konduktometrischer Titration, Elektronen- und IR-Spektrometrie untersucht. Die IR-Daten zeigen, daß die Koordination über N=N, C-OH und Pyridyl erfolgt.

     

从α－蒎烯直接催化酯化高选择性地合成乙酸正龙脑酯的研究－催化剂与反应机理初探

本文提出了新的硼酸类催化剂体系ＨＢ，用该体系对α－蒎烯与无水乙酸相互作用直接合成乙酸正龙脑酯作了较系统的研究。反应得到两种系列产物－酯化产物和异构化产物，酯化产物主要是乙酸正龙脑酯，葑醇酯和松油酯，异构化产物主要是莰烯、烯和松油烯等，总酯化产率为５０％以上，其中乙酸正龙脑酯为２０％以上，是至今从α－蒎烯直接合成乙酸正龙脑酯的最好结果。通过对产物的￣１ＨＮＭＫ图谱分析及动力学考察，确证反应主产物是正龙脑酯而不是异龙脑酯。文章对Ｈ＿２ＳＯ＿４、ＨＣｌＯ＿４、多聚磷酸（ＰＰＡ）和杂多酸（１２－磷钨酸）等催化剂进行了实验考察、对比和评述，表明了自制的ＨＢ催化剂体系具有高选择性合成乙酸正龙脑酯的显著优点，并对其反应机理作了初步探讨。     

Metabolomic-based investigation of Yinlan alleviating hyperlipidemia by inhibiting blood stasis and phlegm turbidity through the PXR-CYP3A4-ABCB1-FXR pathway

Yinlan lipid regulatory capsule (YL) is a composite traditional Chinese medicine (TCM) new drug to alleviate hyperlipidemia, while its therapeutic mechanism in vivo was not clarified with nontargeted metabolomics investigation. An animal model was established in rats fed a high-fat diet, and their body weights, body mass index (BMI) and blood cholesterol levels were measured. Serum, liver and kidney tissue samples were also extracted for PXR-CYP3A4-ABCB1-FXR signaling pathway research using PCR and UHPLC–MS. The obtained plasma samples were analyzed by UHPLC-Q-TOF-MS metabolomic investigation, which revealed PXR-CYP3A4-related metabolites and changes induced by YL. Finally, the key metabolites were chosen as index components, and their levels in the serum, liver, small intestine and bile were used for simultaneous UHPLC–MS-MS determination. The results indicated that YL was effective in rebalancing blood TG and TC levels (compared to controls). With respect to the PXR-CYP3A4-ABCB1 pathway, as a result of YL’s effect, gene expression or activity of the two targets decreased significantly in both the liver and kidney. The same trend was observed in the serum samples mentioned above. Metabolomics screening and data revealed that 44 metabolites can be regarded as biomarkers related to hyperlipidemia, fatty acids synthesis, and body energy consumption, as well as synthesis, transportation and exertion of cholesterol. YL’s treatment focused on 26 of them, primarily bile acids, indicating that the antihyperlipidemic effect of this drug lies in its inhibitory activity of cholesterol metabolism. Subsequent analysis of those in vivo components revealed that significant increases (compared to the model group) occurred in the blood, liver, small intestine and bile in groups that received medium and high doses of YL (while the low dose was relatively unchanged). Those target components exhibit a close relationship with PXR and/or CYP3A4. The use of YL repressed PXR expression and subsequently decreased CYP3A4 activity. As a result, synthesis of related bile acids increased, while cholesterol levels decreased, consequently leading to the attenuation of hyperlipidemia. This study comprehensively investigated the antihyperlipidemia mechanism of YL based on its repression of PXR-CYP3A4 activity and related metabolite yield, establishing an accurate method for evaluating the therapeutic effect of YL.     

Fluorimetric determination of ascorbic acid with o-phenylenediamine

A simple and sensitive fluorimetric method for the determination of ascorbic acid (AA) is described. The method is based on the condensation reaction between AA and o-phenylenediamine (OPDA) in the absence of the oxidant. The fluorescence intensity is measured at excitation and emission wavelengths of 360 and 430 nm, respectively. Under optimum condition, a linear relationship is obtained between the fluorescence intensity and the concentration of AA in the range of 0.05-40 μg ml⁻¹. The detection limit is 0.006 μg ml⁻¹, which is obviously lower than that of other fluorimetric methods reported.     

酸性品红与蛋白质结合反应的研究及应用

在pH1.4的Clark-Lubs缓冲介质中，蛋白质与酸性品红反应形成结合物，该结合物的最大吸收波长为576nm，与酸性品红相比，红移了34nm。据此拟定了分析方法，制定了牛血清白蛋白(BSA)、人血清白蛋白(HAS)、γ-球蛋白(γ-G)和酪蛋白的工作曲线，测定的摩尔吸光系数均在10^5数量级，用于人血清中总蛋白的测定，结果与溴甲酚绿(BCG)法基本一致。     

钙黄绿素蓝荧光法测定食品中的微量锌（Ⅱ）

本文研究了在ＣＴＭＡＢ存在下，用钙黄绿素蓝荧光法测定食品中的微量锌（Ⅱ）的实验条件。在本实验条件下，Ｚｎ（Ⅱ）与钙黄绿素蓝生成１：１的配合物使钙黄绿素蓝的荧光增强，最大激发波长和最大发射波长分别为３５３ｎｍ和４４０ｎｍ。     

重油催化裂化汽油中含氮化合物的分析

利用酸萃取技术浓缩分离重油催化裂化（RFCC）汽油中的氮化物，比较了两种萃取剂和两种油剂比对分离效果的影响，结果发现选用10％（体积分数）HCl作萃取剂，油剂比为10：1（体积比）时，碱性氮化物的提取率较高；浓缩分离出的氮化物用色谱－质谱联用方法对其进行了检测，结果表明RFCC汽油中的氮化物主要是C0－C2苯胺及少量吡啶类、喹啉类碱性氮化物。