应用质量源于设计的理念优化大鼠血浆中大黄蒽醌的分析方法

应用质量源于设计理念建立一种高效液相色谱-荧光检测法(HPLC-FLD)用于测定大鼠血浆中5种大黄蒽醌。用Plackett-Burman设计考察流动相中甲醇含量、pH值、流速、柱温和进样体积对色谱峰的分离度、理论塔板数、最末洗脱峰的保留时间和拖尾因子的影响,结果显示流动相中甲醇含量、流速和柱温对色谱系统的影响显著(p<0.05)。继而采用Box-Behnken设计结合响应面法考察上述三因素对分离度、保留时间和理论塔板数的影响。用Derringer渴求函数评价了响应值的综合作用。得出最优色谱条件为:以甲醇-0.1%(v/v)磷酸水溶液(81.4:18.6, v/v)为流动相等度洗脱,流速1.1 mL/min,柱温31℃,荧光检测激发波长为440 nm,发射波长为540 nm。建立的模型显示良好的预测性。结果表明:质量源于设计的理念可有效地应用于优化高效液相色谱分析方法。     

大黄蒽醌提取物对罗氏沼虾抗高温应激的影响

 将罗氏沼虾随机分成5组,每组3个平行,每个平行约1 000尾,第1组为对照组,投喂基础日粮,另外4组为试验组,在基础日粮中分别添加 w 为0.05%、0.10%、0.20%、0.40%大黄蒽醌提取物。饲养8周后,对虾进行连续48 h 35 ℃高温应激,测定其生长、应激前后血淋巴葡萄糖、胆固醇、甘油三酯、溶菌酶、一氧化氮（NO）等的变化。结果表明：与对照组相比,添加 w=0.10%的大黄蒽醌提取物显著提高了虾的增重率、降低了饵料系数,w=0.40%大黄蒽醌提取物显著增加了血淋巴溶菌酶含量。高温应激后,与对照组相比,添加 w 为0.1%和0.20%大黄蒽醌提取物仍保持较高血淋巴溶菌酶、一氧化氮浓度。高温应激试验表明：对照组死亡率达60%,添加 w为0.10%和0. 20%大黄蒽醌提取物小于30%。因此添加 w 为0.10%和0.20%大黄蒽醌提取物提高了机体抗应激能力,并对高温引起虾的死亡有一定的保护作用,促进了虾的生长。     

超临界流体萃取-胶束电动毛细管色谱法分离测定大黄中蒽醌类组分的含量

采用ＳＴＥ－ＭＥＣＣ法分离测定大黄中的芦荟大黄素，大黄素和大黄酸。萃取条件为压 力４１．４ＭＰａ，温度５０℃，改性剂量０．４ｍＬ。被测组分在１０ｍｉｎ得到全部分离。本法准确、简 便、快速、结果令人满意。     

决明子有效成分的提取

决明子的主要功能化学成分有蒽醌类、吡酮类和多糖等，具有降血脂、降血压、保肝、通便等作用。本文采用乙醇提取决明子中的三种有效成分：多糖、蒽醌、黄酮。对乙醇浓度、浸提温度、浸提时间、固液比、浸提次数进行了单因素梯度实验，确定了其条件范围，通过进一步正交实验得到决明子有效成分的乙醇提取工艺的最优因素组合．乙醇浓度50％，浸提温度60℃，浸提时间2．5h，固液比l：20。     

The cyclization of vicinal 1-amino-2-acylvinylated derivatives of aromatic amines

A general method for the synthesis of substituted fused polycyclic compounds containing a 4-alkylamino or 4-dialkylaminopyridine cycle has been proposed. The method includes the addition of primary or secondary amines to vicinal (acylethynyl)arylamines followed by the cyclization of the adducts under acidic or basic catalysis conditions. Various aminonaphthoquinolinediones and aminoquinolines have been prepared in high yields by this method.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1423–1429, August, 1993.     

GC-MS and LC-MS Identification of the Phenolic Compounds Present in the ethyl Acetate Fraction Obtained from Senna tora,L. Roxb. seeds

The aim of this work is to characterize the active constituents present in the ethyl acetate fraction of Senna tora, L. Roxb. seeds. Due to the fact that the main biological activity of S. tora, L seeds is attributed to its phenolic compounds which are mainly isolated from Ethyl acetate fraction, to avoid repetition of work and to save time, it was deemed necessary to confirm the identity of these phenolic compounds. This was done by GC-MS and LC-MS analysis of the ethyl acetate fraction where the structures of the isolated compounds were established on the basis of molecular ion peak and their fragmentation pattern. They were identified as Chrysophanol, Chrysarobin, 10-hydroxy-5-methoxy-2-methyl-1, 4-anthracenedione, Rubrofusarin, Parietin, Griseoxanthone-B, Isotorachrysone, and Cumbiasin B.

     

Cyclization of 1-hydroxy-2-(oxoalkynyl)anthraquinones

Procedures were developed for the heterocyclization of 2-benzoylethynyl-1-hydroxy-and 1-hydroxy-2-(1-oxo-3-phenylpropynyl)anthraquinone. The regioselective preparation of 2-substituted anthra[1,2-b]pyran-4,7,12-triones was demonstrated to be possible under mild conditions.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2686–2692, December, 2004.     

The study of photoisomerisation of 1-aryloxyanthraquinones by NMR spectroscopy and UV spectrophotometry

It has been stated by ¹H NMR and UV spectrophotometry that 1-(4-tert-butil-phenoxy)-2-cetylamino-9,10-anthraquinone photoisomerizes to 9-(4-tert-butylphenoxy)-2-cetylamino-1,10-anthraquinon with quantum yield ? = 0.4 ±0.1 under light excitation in the absorption band region in the UV/visible spectrum range with the maximum λ = 441 nm.