Fast liquid chromatography for racemic atenolol acetate separation— TT he analytical protocol

机译：外消旋液相色谱法为外消旋乙酸乙酸酯分离 - T T HE分析方案

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Abstract > Kinetic resolution of ( <fi>R</fi> , <fi>S</fi> )‐atenolol is a faster strategy to produce ( <fi>S</fi> )‐atenolol. Since this racemate is a less soluble compound, resolution of its ester offers high concentrations in the process. A good analytical method is required to observe the enantiomer concentrations. This paper described application of ultra‐fast liquid chromatography on the atenolol ester separation using different resolution media and analytical procedures. Chiralcel OD column resolved the ester. The chromatograms indicated different characteristics of the process. The enantiomers could be recognized by the column in less than 1 (one) hour. Symmetrical peaks were obtained, but several procedures produced peaks with wide bases and slanted baselines. Efficient enantioresolution was obtained at high mobile phase flow rate, decreased concentration of amine‐type modifier, but increased alcohol content in the mobile phase. High UV detection wavelength was required. At 1.0?mL/min, the (90/10/0.5) composition resulted <fi>α</fi> ?=?1.46 and <fi>R</fi> <sub> <fi>S</fi> </sub> ?=?0.9998 that were good separation. </abstract> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> <div class="translation abstracttxt"> <span class="zhankaihshouqi fivelineshidden" id="abstract"> <span>机译：</span><Abstract Type =“Main”XML：Lang =“en”> <标题类型=“main”>抽象</ title> >动态分辨率（<fi> r </ fi>，<fi> s </ FI>）-ATENOLOL是生产（<fi> s </ fi>）-ateholol的更快的策略。由于这种外消旋体是一种不太可溶的化合物，因此其酯的分辨率在该过程中提供高浓度。需要良好的分析方法来观察对映体浓度。本文描述了使用不同分辨率培养基和分析方法在阿内洛尔酯分离上施加超快速液相色谱。 Chiralcel OD列分辨酯。色谱图表明该过程的不同特征。对映体可以在小于1（一小时）的柱中识别。获得对称峰，但几种程序产生宽碱和倾斜基线的峰。在高流动相流速下获得高效的对脑溶液，降低胺型改性剂的浓度，但在流动相中增加了醇含量。需要高UV检测波长。在1.0？ml / min，（90/10 / 0.5）组合物得到<fi>α</ fi>？=α1.46和<fi> R </ fi> <sub> <fi> s </ fi> < / sub>？=？0.9998是良好的分离。 </ p> </ abstract> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> </div> <div class="record"> <h2 class="all_title" id="enpatent33" >著录项</h2> <ul> <li> <span class="lefttit">来源</span> <div style="width: 86%;vertical-align: text-top;display: inline-block;"> <a href='/journal-foreign-16290/'>《Chirality: The pharmacological, biological, and chemical consequences of molecular asymmetry》</a> <b style="margin: 0 2px;">|</b><span>2017年第12期</span><b style="margin: 0 2px;">|</b><span>共7页</span> </div> </li> <li> <div class="author"> <span class="lefttit">作者</span> <p id="fAuthorthree" class="threelineshidden zhankaihshouqi"> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Agustian Joni&option=202" target="_blank" rel="nofollow">Agustian Joni;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Kamaruddin Azlina Harun&option=202" target="_blank" rel="nofollow">Kamaruddin Azlina Harun;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Aboul‐Enein Hassan Y.&option=202" target="_blank" rel="nofollow">Aboul‐Enein Hassan Y.;</a> </p> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zkzz" style="display: none;">展开▼</span> </div> </li> <li> <div style="display: flex;"> <span class="lefttit">作者单位</span> <div style="position: relative;margin-left: 3px;max-width: 639px;"> <div class="threelineshidden zhankaihshouqi" id="fOrgthree"> <p>Department of Chemical EngineeringUniversitas LampungBandar Lampung Lampung Indonesia;</p> <p>School of Chemical Engineering Engineering CampusUniversiti Sains MalaysiaPenang Malaysia;</p> <p>Pharmaceutical and Medicinal Chemistry Department Pharmaceutical and Drug Industries DivisionNational Research CentreCairo Egypt;</p> </div> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zhdw" style="display: none;">展开▼</span> </div> </div> </li> <li > <span class="lefttit">收录信息</span> <span style="width: 86%;vertical-align: text-top;display: inline-block;"></span> </li> <li> <span class="lefttit">原文格式</span> <span>PDF</span> </li> <li> <span class="lefttit">正文语种</span> <span>eng</span> </li> <li> <span class="lefttit">中图分类</span> <span><a href="https://www.zhangqiaokeyan.com/clc/4812.html" title="结构化学">结构化学;</a></span> </li> <li class="antistop"> <span class="lefttit">关键词</span> <p style="width: 86%;vertical-align: text-top;"> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=atenolol&option=203" rel="nofollow">atenolol;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=C hiralcel OD&option=203" rel="nofollow">C hiralcel OD;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=enantiomers separation&option=203" rel="nofollow">enantiomers separation;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=kinetic resolution&option=203" rel="nofollow">kinetic resolution;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=ultra‐fast liquid chromatography&option=203" rel="nofollow">ultra‐fast liquid chromatography;</a> </p> <div class="translation"> 机译：atenolol;c hiralcelod;对映体分离;动力学分辨率;超快速液相色谱; 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href="/academic-journal-cn_chemical-enterprise-management_thesis/0201246824274.html">无水乙酸+乙酸酐对L-脯氨酸的消旋探究</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=邵喆&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 邵喆</a> <span> <a href="/journal-cn-9143/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 化工管理 </a> </span> <span> . 2018</span><span>,第024期</span> </span> </div> </li> <li> <div> <b>5. </b><a class="enjiyixqcontent" href="/academic-journal-cn_journal-instrumental-analysis_thesis/0201230593842.html">支链淀粉-三(苯基氨基甲酸酯)手性固定相的制备及酸性外消旋药物联苯双酯的拆分</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=周志强&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 周志强</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=丁二润&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,丁二润</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=侯经国&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,侯经国</a> <span> <a href="/journal-cn-10803/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 分析测试学报 </a> </span> <span> . 1998</span><span>,第005期</span> </span> </div> </li> <li> <div> <b>6. </b><a class="enjiyixqcontent" href="/academic-conference-cn_meeting-58765_thesis/020222545841.html">混合溶剂重结晶法分离内消旋与外消旋2,3-二氰基-2,3-二苯基丁二酸二乙酯及理论分析</a> <b>[C]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=黄红军&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 黄红军</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=闫军&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,闫军</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=张文宇&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,张文宇</a> <span> <a href="/conference-cn-58765/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 中国化学会2000年学术会议 </a> <span> <span> . 2000</span> </span> </div> </li> <li> <div> <b>7. </b><a class="enjiyixqcontent" href="/academic-degree-domestic_mphd_thesis/020313507027.html">分子内芳基乙酸型重氮酯与内消旋二叠氮丙醇的去对称化反应研究</a> <b>[A] </b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=乔金宝&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 乔金宝</a> <span> . 2016</span> </span> </div> </li> </ul> <ul style="display: none;"> <li> <div> <b>1. </b><a class="enjiyixqcontent" href="/patent-detail/06120105293004.html">(外消旋)－乙酸－1－(乙酰氧基苯基)－3－烯－1－丁酯的制备方法</a> <b>[P]</b> . <span> 中国专利： CN101092356A </span> <span> . 2007-12-26</span> </div> </li> <li> <div> <b>2. </b><a class="enjiyixqcontent" href="/patent-detail/06120555598.html">外消旋－二有机甲硅烷基双(2－甲基苯并[e]茚基)锆化合物的外消旋选择性合成</a> <b>[P]</b> . <span> 中国专利： CN100558737C </span> <span> . 2009.11.11</span> </div> </li> <li> <div> <b>3. </b><a class="enjiyixqcontent" href="/patent-detail/06130415182870.html">Separation process of a mixture comprising HF and HFC - 1234yf, separation process of HFC - 1234yf a mixture comprising hydrogen fluoride and the mentioned this 1234yf, separation process of hydrogen fluoride in a mixture comprising hydrogen fluoride and HF. C - 1234yf, purification process of HFC - 1234yf from a mixture comprising HFCS - 1234yf and HF.Purification process of HF from a mixture comprising an HFC - 1234yf and HF, separation of a mixture of HFC - 1234yf HFC - 1234yf, HF and at least one of HFC - 245cb or HFCS - 245eb and separation process of a mixture comprising HF HFC - 1234yf, HF and at least u M of HFC - 245cb or HFCS - 245eb</a> <b>[P]</b> . <span> 外国专利：  BRPI0906014A2 </span> <span> . 2015-06-30</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：包含HF和HFC的混合物的分离过程-1234yf，HFC-1234yf的分离过程，包含氟化氢和上述的1234yf的混合物，包含氟化氢和HF的混合物中的氟化氢的分离过程。 C-1234yf，从包含HFCS-1234yf和HF的混合物中纯化HFC-1234yf的过程。从HFC-1234yf和HF的混合物中纯化HF，分离HFC-1234yf的混合物HFC-1234yf，HF和HFC-245cb或HFCS-245eb中的至少一种以及包含HF HFC-1234yf，HF和至少1 M的HFC-245cb或HFCS-245eb的混合物的分离方法 </span> </p> </li> <li> <div> <b>4. </b><a class="enjiyixqcontent" href="/patent-detail/06130415182869.html">"process for separating a mixture comprising hf and hfc-1234ze, process for separating an e-hfc-1234ze from a mixture including hydrogen fluoride and said e-hfc-1234ze, process for separating" of hydrogen fluoride from a mixture containing hydrogen fluoride and e-hfc-1234ze, process for purifying an e-hfc-1234ze from a mixture of e-hfc-1234ze and hf, process for purifying hf from a mixture comprising e-hfc-1234ze and hf, process for separating e-hfc-1234ze from a mixture of e-hfc-1234ze, hf and at least one of hfc-245fa or hfc-245eb and process for hfc-1234yf separation from hfc-1234ze "</a> <b>[P]</b> . <span> 外国专利：  BRPI0906015A2 </span> <span> . 2015-06-30</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：从包含氟化氢的混合物中分离氟化氢的“分离包含hf和hfc-1234ze的混合物的方法，从包含氟化氢和所述e-hfc-1234ze的混合物中分离e-hfc-1234ze的过程，分离方法”。 e-hfc-1234ze，从e-hfc-1234ze和hf的混合物中纯化e-hfc-1234ze的方法，从包含e-hfc-1234ze和hf的混合物中纯化hf的方法，分离e-hfc-从e-hfc-1234ze，hf和hfc-245fa或hfc-245eb中至少一种的混合物中提取1234ze，以及从hfc-1234ze中分离hfc-1234yf的方法 </span> </p> </li> <li> <div> <b>5. </b><a class="enjiyixqcontent" href="/patent-detail/06130425478771.html">The azeotropic or near azeotropic composition, processes for the separation of Z - HFC - 1225ye, a process for the purification of Z - HFC - 1225ye, process for the production of Z - HFC - 1225ye and process for the separation of HFC - 236ea</a> <b>[P]</b> . <span> 外国专利：  BRPI0619645A2 </span> <span> . 2011-10-04</span> </div> <p class="zwjiyix translation" style="max-width: initial;height: auto;word-break: break-all;white-space: initial;text-overflow: initial;overflow: initial;"> <span>机译：共沸或近共沸组成，Z-HFC-1225ye的分离方法，Z-HFC-1225ye的纯化方法，Z-HFC-1225ye的生产方法和HFC-236ea的分离方法 </span> </p> </li> </ul> </div> </div> </div> <div class="theme cardcommon" style="overflow: auto;display:none"> <h3 class="all_title" 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