5-乙巯基四氮唑质量标准研究  

Study on Quality Control for 5-Ethylthio-1H-Tetrazole

作　　者：仲婕 李保山 鲁丹丹[2] 朱德领 张金钟 马金平 金艳 

机构地区：[1]杭州天龙药业有限公司,杭州310021 [2]军事医学科学院放射与辐射医学研究所,北京100850

出　　处：《中国药品标准》2013年第3期208-211,共4页Drug Standards of China

基　　金："十二五"国家重大新药创制科技重大专项(2011ZX09102-001-07;2011ZX09102-009-09)

摘　　要：目的:对寡核苷酸固相合成所用活性基团保护剂5-乙巯基四氮唑进行质量(纯度)控制。方法:薄层色谱法和反相离子对高效液相色谱法。在硅胶GF254薄层板上,建立二氯甲烷-甲醇-丙酮-三乙胺(6∶1∶1∶0.2)薄层分离体系;在Diamonsil C18(4.6 mm×250 mm,5μm)色谱柱上,以甲醇-乙腈-水(含0.06%硫酸,0.5%硫酸钠和0.02%庚烷磺酸钠)(16∶16∶68)为流动相,建立液相色谱分离体系,检测波长224nm。结果:水分控制在0.5%以下,纯度控制在大于等于98%,才能保证活化和缩合反应完全。结论:所建立的方法准确,限度合理,能保证合成用5-乙巯基四氮唑的纯度。Objective： To control 5-ethylthio-lH-tetrazole quality （purity） which is one of the most important active intermediate , as a activator for condensation in solid-phase synthesis of oligonucleotide. Methods： Thin-layer chromatography （TLC） and ion pair re-versed-phase high performance liquid chromatography （IP-HPLC） were studied in this article. To establish the system of dichlorometh-ane-methanol-acetone-triethylamine （6： 1： 1： 0. 2） on silica gel GF254plate, perform a HPLC method on a Diamonsil Cls （4.6mm×250mm,5μm） column with methanol-acetonitrile-water （containing 0. 06% sulfuric acid, 0. 5% sodium sulfate and 0. 02% sodium heptanesulfonate） （ 16： 16：68 ）as mobile phase, detection wavelength was 224nm. Results： To ensure a complete activation and con-densation reaction, by means of moisture control within 0. 5% and purity control not less than 98% for activator , 5-ethyhhio-1H-tet- razole, were useful in the processing of synthesis. Conclusions： The methods are accurate and the limits are reasonable, had been used in tracking down the quality of 5-ethyhhio-1H-tetrazole in oligonucleotide synthesis event.

关 键 词：寡核苷酸合成 5-乙巯基四氮唑 质量标准 纯度 

分 类 号：R921.2[医药卫生—药学]