Toward breast cancer resistance protein (BCRP) inhibitors: design, synthesis of a series of new simplified fumitremorgin C analogues

In this study, we report the design and synthesis of a series of new simplified fumitremorgin C analogues. The preliminary biological study indicated some of these simplified fumitremorgin C might be developed into breast cancer resistance inhibitors.     

A New Asterosaponin from the Starfish Culcita novaeguineae

A new asterosaponin named novaeguinoside A, along with a known saponin, asteronyl pentaglycoside sulfate, was isolated from the starfish Culcita novaeguineae. The new compound was identitied to be sodium 6α-O-{β-D-fucopyranosyl-(1→2)-β-D-fucopyranosyl-(1→4)-[β-D-quinovopyranosyl-(1→2)]-β-D-xylopyranosyl-(1→3)-[β-D-quinovopyranosyl}-5α-pregn-9(11)-en-20-one-3β-yl-sulfate by extensive spectral analysis and chemical evidence.     

2-芳基硫杂脯氨酸结构特征的研究

对12种2-芳基硫杂脯氨酸进行了红外光谱和核磁共振谱测定,对其中两个化合物作了质谱测定。结果表明,这类化合物固态时主要以两性离子形式存在;有较强的分子离子峰,是一类较稳定的化合物。它们还存在一对非对映异构体,芳环上的取代基对芳环电子云密度的影响较大,而对四氢噻唑环的影响较小。     

尿中肌酐的流动注射分析

本文提出了一种简便快速的尿中肌酐的测定方法。采用空气整段间隔试样带的流动注射分析体系,在非化学反应平衡的条件下测定,尿样不经手工稀释可直接用于测定。测样频率每小时为90次,相对标准偏差为1.5%。     

SrZnO_2∶Eu~(3+),Li~+长波紫外激发红光荧光体的合成及发光性能研究

采用高温固相法合成了一种长波紫外激发的SrZnO2∶Eu3+,Li+发光材料,用X射线衍射谱、荧光光谱对样品进行了表征。结果表明,Eu3+离子在SrZnO2基质中主要占据Sr2+离子不对称性格位,发射来源于5D0→7F2612 nm为主的红光。加入电荷补偿剂Li+离子能显著提高发光强度,350~400 nm内的激发峰也有明显提高,同时观察到来自Eu3+离子高能级5D1→7FJ(J=0~2)的跃迁发射,并对其产生机制进行了初步探讨。实验结果表明,SrZnO2∶Eu3+,Li+是一种有发展前途的长波紫外激发红光荧光体。     

In-channel indirect amperometric detection of nonelectroactive anions for electrophoresis on a poly(dimethylsiloxane) microchip

In the present paper, we describe a microfluidics-based sensing system for nonelectroactive anions under negative separation electric field by mounting a single carbon fiber disk working electrode (WE) in the end part of a poly(dimethylsiloxane) microchannel. In contrast to work in a positive separation electric field described in our previous paper (Anal. Chem. 2004, 76, 6902-6907), here the electrochemical reduction reaction at the WE is not coupled with the separation high-voltage (HV) system, whereas the electrochemical oxidation reaction at the WE is coupled with the separation HV system. The electroactive indicator is the carbon fiber WE itself but not dissolved oxygen. This provides a convenient and sensitive means for the determination of nonelectroactive anions by amperometry. The influences of separation voltage, detection potential, and the distance between the WE and the separation channel outlet on the response of the detector have been investigated. The present detection mode is successfully used to electrochemically detect F-, Cl-, SO4(2-), CH3COO-, H2PO4-. Based on the preliminary results, a detection limit of 2 microM and a dynamic range up to three orders of magnitude for Cl- could be achieved.     

Determination of the Enantiomeric Purity of l-Carnitine and Acetyl-l-Carnitine by Chiral Liquid Chromatography

A chiral liquid chromatographic method for determination of the enantiomeric purity of both l-carnitine and acetyl-l-carnitine is described. Separation of the enantiomers of dl-carnitine and acetyl-dl-carnitine was achieved on a commercial chiral column (Chiralcel OD-R) after derivatization with (alpha-bromo)methyl phenyl ketone. Introduction of this lipophilic UV chromophoric group to the carnitine and acetylcarnitine molecules improved their retention, resolution, and UV detection. The mobile phase was 74:26 (v/v) 0.5 mol L^-1 sodium perchlorate–acetonitrile, pH 3.8, and the flow rate was 0.4 mL min^-1. Detection was performed at 235 nm. The method is selective and reliable for determination of the enantiomeric purity of bulk drug substances l-carnitine and acetyl-l-carnitine.     

同时测定食用植物油中抗氧剂叔丁基对羟基茴香醚和2，6－二叔丁基对甲酚的方法

报道了用高效液用色谱法同时测定食用植物油中的抗氧剂叔丁基对羟基茴香醚（ＢＨＡ）和２，６－二叔丁基对甲酚（ＢＨＴ）的实验方法。采用ＺｏｒｂａｘＯＤＳＣ_（１８）色谱住，甲醇：水（９０：１０，Ｖ／Ｖ）作流动相，检测波长为２４５ｎｍ，流速为１ｍＬ／ｍｉｎ。检测下限分别为１５ｎｇ（ＢＨＡ），９０ｎｇ（ＢＨＴ），回收率分别是９６．８％±９．８％（ＢＨＡ），９９．０％±３．２％（ＢＨＴ）。方法快速、准确，灵敏度高。     

Electrothermal volatilization of aluminum as 1-phenyl-3-methyl-4-benzoylpyrazolone[5] chelate for gaseous sample introduction in ICP-AES

Based on gaseous compound introduction as 1-phenyl-3-methyl-4-benzoylpyrazolone[5](PMBP) chelate of aluminum by electrothermal vaporization in ICP-AES, a method for determination of trace aluminum was developed. Trace aluminum was vaporized at temperature of 1000 degrees C, and the vaporization behavior of aluminum chelate was detailedly investigated. Under the optimum conditions, the detection limit of aluminum was 0.6 ng ml(-1), and the relative standard deviation for 0.1 mug ml(-1) aluminum was 4.7% (n=8). The proposed method was applied to the determination of trace aluminum in rice flour reference materials, and the results well agreed with the reference values.     

溶剂萃取法制备碳酸盐的热力学讨论

向金属氯化物(Ⅰ)的水溶液中通入CO_2气体,以期制备相应的碳酸盐和酸式碳酸盐,在常温常压下,体系的△G>0,反应几乎是不可能的。向反应体系中加入有机溶剂(S),使生成的HCl即被萃取,可促进Ⅰ的继续转化。分析计算表明,S对HCl必须有很强的萃取能力,其K_萃须在10~5以上。研究了加入有机溶剂N_(235)前后,体系的热力学状态、函数及其变化。加入N_(235)后,K_萃值增大了5个数量级。考察了温度、时间和通气次数对系统热力学性质的影响。根据反应的耦合原理和热力学分析,提出萃取剂选择的原则。结合实验数据的估算说明:溶剂萃取法由Ⅰ和CO_2制备碳酸盐的工艺路线是可行的。