Column chromatography of human embryonic hemoglobins

Summary Hemoglobin components of human embryonic red blood cells obtained from intact embryos of 20 and 40 mm crown-rump length could be separated by column chromatography on DEAE-Sephacel. The isolation of Hb Gower 1, Hb Gower 2, Hb Portland, Hb F, Hb F₁, and Hb A is possible by this method. In the smaller embryos with only 30% of fetal hemoglobin Hb Gower 1 is the predominant component, whereas in the larger ones with 61% of fetal hemoglobin more Hb Gower 2 than Hb Gower 1 is found.     

头孢拉定原料及制剂的聚合物杂质分析#br#

目的 建立头孢拉定原料及制剂中聚合物杂质的分析方法。方法 采用碱降解法制备头孢拉定强制降解溶液;采用高效凝胶色谱法(TSK G2000 SWxl)和柱切换-LC/MS法对头孢拉定强制降解溶液中的聚合物杂质进行分离和结构鉴定;采用Agilent ZORBAX SB-C18型色谱柱,以磷酸盐缓冲液-甲醇为流动相,进行梯度洗脱,建立头孢拉定聚合物的RP-HPLC分析方法,采用二维液相色谱法和柱切换-LC/MSn法对该方法的专属性进行分析;进行方法学验证。结果 在头孢拉定强制降解物中鉴定出头孢拉定二聚体、三聚体、四聚体;高效凝胶色谱法分离头孢拉定聚合物杂质时,易受到小分子杂质的干扰,同时分离的聚合物杂质色谱峰拖尾严重,存在肩峰,定量准确性差;RP-HPLC法分析头孢拉定聚合物杂质时,在20~22min范围内检出头孢拉定二聚体、三聚体、四聚体;方法定量限为500μg,最低检测限为150μg。结论 高效凝胶色谱法不能对头孢拉定中的聚合物杂质进行有效质控,建立的反相色谱法分析头孢拉定聚合物杂质时专属性良好、灵敏度高、方法耐用性好,可用于头孢拉定原料及制剂的聚合物杂质质控;头孢拉定强制降解溶液可作为头孢拉定聚合物分析的系统适用性溶液。     

A systematic stability evaluation of analytical RP-HPLC columns

HPLC column stability is one of the critical factors that determine the success of a method while supporting the life cycle of a pharmaceutical product. A systematic approach for the evaluation of HPLC column stability has been developed with emphasis on the practicality of the application to pharmaceutical analysis. This paper describes the specifics of the experimental design, evaluation criteria used and result obtained for some of the most widely used analytical columns from highly reputable column manufacturers. A stability profile over the most commonly used pH range was established that may serve as a reference for column scouting during method development.     

用RhD阳性红细胞从含抗D抗体的IgG中提纯抗D抗体

目的：研究从含抗-D抗体的IgG中纯化抗D抗体的方法。方法：抗D含量为0.814μg/ml的健康人血浆,经柱层析法分离获得含抗D的IgG后,用遗传表现型CCDee的RhD阳性＂O＂型红细胞经亲和层析法从IgG中纯化抗-D抗体。检测相关指标。结果：经过亲和层析法纯化后去除了近90%的非目的IgG,使产物可以进一步浓缩以提高单位体积制剂中抗-D抗体浓度。所得制剂经检测各项指标均符合中国生物制品规程的要求。结论：本方法可从含抗D的IgG制剂中进一步纯化抗D抗体,为血浆综合利用提供参考。     

Oxidation Potentials of Flavonoids Determined by Flow-through Column Electrolysis

1　ＩｎｔｒｏｄｕｃｔｉｏｎＦｌａｖｏｎｏｉｄｓａｒｅｎａｔｕｒａｌｃｏｍｐｏｕｎｄｓ ,ｗｉｄｅｌｙｄｉｓｔｒｉｂｕｔｅｄｉｎｆｒｕｉｔｓ,ｖｅｇｅｔａｂｌｅｓ,ａｎｄｔｅａｓ.Ｔｈｅｒｅｉｓａｎｉｎｃｒｅａｓｉｎｇｉｎｔｅｒｅｓｔｉｎｔｈｅｓｅｃｏｍｐｏｕｎｄｓｂｅｃａｕｓｅｏｆｔｈｅｉｒｂｒｏａｄ ｐｈａｒｍａｃｏｌｏｇｉｃａｌａｃｔｉｖｉ ｔｉｅｓ ,[1,2 ] ｅｓｐｅｃｉａｌｌｙｔｈｅｉｒａｎｔｉｏｘｉｄａｎｔａｃｔｉｖｉｔｙ .[3～ 5 ] Ａｓａｎｔｉｏｘｉｄａｎｔｓ ,ｆｌａｖｏｎｏｉｄｓｈａｖｅｔｈｅａｂｉｌｉｔｙｔｏｓｃａｖｅｎｇｅｆｒｅｅｒａｄｉｃａｌｓｂｙｐｒｏｔｅｉｎａｎｄｅｌｅｃｔｒｏｎｔｒａｎｓｆｅｒｐｒｏｃｅｓｓｅｓ.Ｏｎｔｈｅｏｔｈｅｒｈａｎｄ ,ａｓｍｅｔａｌ ｃｈｅｌａｔｉｎｇａｇｅｎｔｓ ,ｆｌａｖｏｎｏｉｄｓｃａｎｄｅｐｒｅｓｓｔｈｅｓｕｐｅｒｏｘｉｄｅ ｄｒｉｖｅｎＦｅｎｔｏｎｒｅａｃｔｉｏｎ .[6 ] Ｔｈｅｒｅａｒｅａｌｓｏｒｅｐｏｒｔｓｏｆｆｌａｖｏｎｏｉｄｓｉｎｈｉｂｉｔｉｎｇｔｈｅａｃｔｉｖｉｔｉｅｓｏｆａｎａｒｒａｙｏｆｅｎｚｙｍｅｓ.[1,7,...     

Analysis of an anti-inflammatory steroidal drug,difluprednate, in aqueous humor by combination of semi-micro HPLC and column switching method

A specific and sensitive method for the determination for difluprednate (DFBA) and its metabolite (deacetylated DFBA, DFB) in aqueous humor was developed. DFBA and DFB were initially absorbed on a Pinkerton-type column, then analyzed by high-performance liquid chromatography using a semi-micro column after column switching. Under the optimized conditions, calibration curves for DFBA and DFB showed good linearity over the range of 1.0–50 and 0.5–50 ng/ml, respectively. We applied the method to the analysis of DFBA and DFB in rabbit aqueous humor, and found that DFBA in rabbit aqueous humor 1 h after instillation of 0.002% DFBA ophthalmic emulsion was not detected, but DFB was present at the concentration of 4.3±3.1 ng/ml.     

Bioactive Lignans from Zanthoxylum alatum Roxb. stem bark with cytotoxic potential

Ethanopharmacological relevance

Zanthoxylum alatum is used in traditional medicinal systems for number of disorders like cholera, diabetes, cough, diarrhea, fever, headache, microbial infections, toothache, inflammation and cancer. The aim of the present study was to evaluate Zanthoxylum alatum stem bark for its cytotoxic potential and to isolate the bioactive constitiuents.

Material and methods

Cytotoxicity of the different extracts and isolated compounds was studied on lung carcinoma cell line (A549) and pancreatic carcinoma cell line (MIA-PaCa) using MTT assay. Isolation of compounds from most active extract (petroleum ether) was done on silica gel column. Structure elucidation was done by using various spectrophotometric techniques like UV, IR, ¹H NMR, ¹³C NMR and mass spectroscopy. The type of cell death caused by most active compound C was explored by fluorescence microscopy using the acridine orange/ethidium bromide method.

Result

Petroleum ether extract of plant has shown significant cytotoxic potential. Three lignans sesamin (A), kobusin (B), and 4'O demethyl magnolin (C) has been isolated. All lignans showed cytotoxic activities in different ranges. Compound C was the novel bioactive compound from a plant source and found to be most active. In apoptosis study, treatment caused typical apoptotic morphological changes. It enhances the apoptosis at IC₅₀ dose (21.72 µg/mL) however showing necrotic cell death at higher dose after 24 h on MIA-PaCa cell lines.

Conclusion

Petroleum ether extract (60–80 °C) of Zanthoxylum alatum has cytotoxic potential. The lignans isolated from the petroleum ether extract were responsible for the cytotoxic potential of the extract. 4'O demethyl magnolin was novel compound from Zanthoxylum alatum. Hence the Zanthoxylum alatum can be further explored for the development of anticancer drug.     

Fixed-bed column study for removal of phenol by neem leaves – Experiment,MLR and ANN analysis

This research aims to carry out the column study to remove toxic phenol by natural adsorbent neem leaves (Azadirachta indica). The adsorbent was characterized through SEM, XRD, FTIR, and BET. The phenol removal was performed in the fixed-bed column at optimum pH 3 and room temperature with the change of process variables, i.e., bed height (8.5–13.5 cm), flow rate (10–30 ml/min), and phenol content (100–300 mg/L). These experiments revealed that the breakthroughs of phenol occurred faster for lesser bed height, higher flow rate, and higher phenol content. The Yen et al. model is the best fitted kinetic model and is applicable for scale-up design. The DFT shows that the interaction between different components of the adsorbent and phenol. The artificial neural networks (ANN) modeling using a single hidden layered neural network is successful with the Levenberg-Marquardt algorithm. Desorption of phenol and safe disposal from the used adsorbents were reported.     

学术期刊编辑出版中的人文精神

目的 探讨学术期刊承载的人文功能,体现学术期刊的人文精神。方法 文献研究法,个案研究法。结果 学术期刊体现人文精神的手段有：设置人文栏目、在编排过程中的细节处理及与作者的个性化沟通等。结论 学术期刊承担着传播学术知识,交流学术观点的职能,同时,学术期刊的人文价值也应得到挖掘。