Comprehensive analysis by liquid chromatography Q‐Orbitrap mass spectrometry: Fast screening of peptides and organic molecules

Sardela V. F.; Martucci M. E. P.; Araújo A. L. D.; Leal E. C.; Oliveira D. S.; Carneiro G. R. A.; Deventer K.; Van Eenoo P.; Pereira H. M. G.; Aquino Neto F. R.

摘要

Abstract > The number of substances nominally listed in the prohibited list of the World Anti‐Doping Agency increases each year. Moreover, many of these substances do not have a single analytical target and must be monitored through different metabolites, artifacts, degradation products, or biomarkers. A new analytical method was developed and validated for the simultaneous analysis of peptides and organic molecules using a single sample preparation and LC‐Q‐HRMS detection. The simultaneous analysis of 450 target molecules was performed after cleanup on a mixed‐mode solid‐phase extraction cartridge, combined with untreated urine. The cleanup solvent and reconstitution solvent were the most important parameters for achieving a comprehensive sample preparation approach. A fast chromatographic run based on a multistep gradient was optimized under different flows; the detection of all substances without isomeric coelution was achieved in 11?minutes, and the chromatographic resolution was considered a critical parameter, even in high‐resolution mass spectrometry detection. The mass spectrometer was set to operate by switching between positive and negative ionization mode for FULL‐MS, all‐ion fragmentation, and FULL‐MS/MS 2 . The suitable parameters for the curved linear trap (c‐trap) conditions were determined and found to be the most important factors for the development of the method. Only FULL‐MS/MS 2 enables the detection of steroids and peptides at concentrations lower than the minimum required performance levels set by World Anti‐Doping Agency (1?ng?mL ?1 ). The combination of the maximum injection time of the ions into the c‐trap, multiplexing experiments, and loop count under optimized conditions enabled the method to be applied to </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 XMLNS =“http://www.wiley.com/namespaces/wiley”type =“main”xml：lang =“en”> <title type =“main”>抽象</ title> >数字在禁止的世界反兴奋机构禁止名单中名义上市的物质每年增加。此外，许多这些物质没有单一的分析靶标，必须通过不同的代谢物，伪像，降解产物或生物标志物监测。开发了一种新的分析方法，并验证了使用单个样品制备和LC-Q-HRMS检测同时分析肽和有机分子的同时分析。在混合模式固相萃取盒上清洗后进行450个靶分子的同时分析，与未经处理的尿液结合。清洁溶剂和重构溶剂是实现综合样品制备方法的最重要参数。基于多步梯度的快速色谱运行在不同流动下进行了优化;在11？分钟内实现了没有异常凝胶的所有物质的检测，并且即使在高分辨率质谱检测中，色谱分辨率也被认为是关键参数。通过切换全MS，全离子碎片和全MS / MS <SUP> 2 </ SUP>之间的正极和负电离模式，将质谱仪设定为通过切换正极和负电离模式。确定弯曲线性捕集器（C-Trap）条件的合适参数，发现是该方法开发的最重要因素。只有全MS / MS 2 </ sup>使得能够在浓度低于世界抗掺杂机构设定的最低所需性能水平的浓度下检测类固醇和肽（1？ng？ml α1</ sup>）。在优化条件下，离子的最大喷射时间的最大喷射时间与C-Trap，多路复用实验和环路计数使得能够应用该方法 </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-34906/'>《Journal of mass spectrometry: JMS》</a> <b style="margin: 0 2px;">|</b><span>2018年第6期</span><b style="margin: 0 2px;">|</b><span>共28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=Sardela V. F.&option=202" target="_blank" rel="nofollow">Sardela V. F.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Martucci M. E. P.&option=202" target="_blank" rel="nofollow">Martucci M. E. P.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Araújo A. L. D.&option=202" target="_blank" rel="nofollow">Araújo A. L. D.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Leal E. C.&option=202" target="_blank" rel="nofollow">Leal E. C.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Oliveira D. S.&option=202" target="_blank" rel="nofollow">Oliveira D. S.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Carneiro G. R. A.&option=202" target="_blank" rel="nofollow">Carneiro G. R. A.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Deventer K.&option=202" target="_blank" rel="nofollow">Deventer K.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Van Eenoo P.&option=202" target="_blank" rel="nofollow">Van Eenoo P.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Pereira H. M. G.&option=202" target="_blank" rel="nofollow">Pereira H. M. G.;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Aquino Neto F. R.&option=202" target="_blank" rel="nofollow">Aquino Neto F. R.;</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>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</p> <p>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</p> <p>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</p> <p>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</p> <p>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</p> <p>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</p> <p>Microbiology and ImmunologyGhent University (UGent) Department of Clinical ChemistryTechnologiepark 30 B‐9052 DoCoLab Ghent Belgium;</p> <p>Microbiology and ImmunologyGhent University (UGent) Department of Clinical ChemistryTechnologiepark 30 B‐9052 DoCoLab Ghent Belgium;</p> <p>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</p> <p>Instituto de Química LBCD‐LADETECUniversidade Federal do Rio de JaneiroAvenida Horácio Macedo no. 1281 Polo de Química bloco C Cidade Universitária 21941‐598 Rio de Janeiro RJ Brazil;</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/1187.html" title="分析化学">分析化学;</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=anti‐doping control&option=203" rel="nofollow">anti‐doping control;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=fast comprehensive analysis&option=203" rel="nofollow">fast comprehensive analysis;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=high‐resolution mass spectrometry&option=203" rel="nofollow">high‐resolution mass spectrometry;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Olympic Games&option=203" rel="nofollow">Olympic Games;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Q‐Exactive&option=203" rel="nofollow">Q‐Exactive;</a> </p> <div class="translation"> 机译：防掺杂控制;快速综合分析;高分辨率质谱;奥运会;Q-辐射; </div> </li> </ul> </div> </div> <div class="literature cardcommon"> <div class="similarity "> <h3 class="all_title" id="enpatent66">相似文献</h3> <div class="similaritytab clearfix"> <ul> <li class="active" >外文文献</li> <li >中文文献</li> <li >专利</li> </ul> </div> <div class="similarity_details"> <ul > <li> <div> <b>1. </b><a class="enjiyixqcontent" href="/journal-foreign-detail/0704025633323.html">Comprehensive analysis by liquid chromatography Q‐Orbitrap mass spectrometry: Fast screening of peptides and organic molecules</a> <b>[J]</b> . <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Sardela V. 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href="/journal-cn-7072/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 广东饲料 </a> </span> <span> . 2010</span><span>,第010期</span> </span> </div> </li> <li> <div> <b>2. </b><a class="enjiyixqcontent" href="/academic-journal-cn_journal-anhui-agricultural-sciences_thesis/0201291125522.html">超高效液相色谱-串联质谱法快速测定毒蕈中6种鹅膏毒肽类和鬼笔毒肽类毒素</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=薛康&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 薛康</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=胡江涛&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,胡江涛</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=俞凌云&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,俞凌云</a> <span> <a href="/journal-cn-7281/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 安徽农业科学 </a> </span> <span> . 2021</span><span>,第017期</span> </span> </div> </li> <li> <div> <b>3. </b><a class="enjiyixqcontent" href="/academic-journal-cn_chinese-journal-analytical-chemistry_thesis/0201230581320.html">超高效液相色谱三重四极杆质谱联用法快速检测尿液和血浆中鹅膏毒肽和鬼笔毒肽</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=张秀尧&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 张秀尧</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=蔡欣欣&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,蔡欣欣</a> <span> <a href="/journal-cn-10804/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 分析化学 </a> </span> <span> . 2010</span><span>,第001期</span> </span> </div> </li> <li> <div> <b>4. </b><a class="enjiyixqcontent" href="/academic-journal-cn_chinese-journal-chromatography_thesis/0201288568716.html">TurboFlow在线净化-液相色谱-串联质谱法快速检测人尿中鹅膏肽类毒素</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=方为&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 方为</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=邱凤梅&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,邱凤梅</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=余新威&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,余新威</a> <span> <a href="/journal-cn-14390/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 色谱 </a> </span> <span> . 2021</span><span>,第003期</span> </span> </div> </li> <li> <div> <b>5. </b><a class="enjiyixqcontent" href="/academic-journal-cn_quality-safety-agro-products_thesis/0201279973875.html">高效液相色谱-串联质谱法快速测定小龙虾中去甲万古霉素和杆菌肽</a> <b>[J]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=赵静&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 赵静</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=杨艳&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,杨艳</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=马华&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,马华</a> <span> <a href="/journal-cn-6792/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 农产品质量与安全 </a> </span> <span> . 2020</span><span>,第006期</span> </span> </div> </li> <li> <div> <b>6. </b><a class="enjiyixqcontent" href="/academic-conference-cn_meeting-22338_thesis/02022599983.html">液相色谱-质谱联用法快速筛选苔类粗提液中双联苄化合物</a> <b>[C]</b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=吕蓓蓓&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 吕蓓蓓</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=邢杰&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,邢杰</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=谢春锋&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor">,谢春锋</a> <span> <a href="/conference-cn-22338/" target="_blank" rel="nofollow" class="tuijian_authcolor"> . 中国有机质谱学第十四届全国学术大会 </a> <span> <span> . 2007</span> </span> </div> </li> <li> <div> <b>7. </b><a class="enjiyixqcontent" href="/academic-degree-domestic_mphd_thesis/020315126111.html">Q-Orbitrap高分辨质谱检测中药中非法添加的合成色素和补肾壮阳类化学药物</a> <b>[A] </b> <span> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=李可&option=202" target="_blank" rel="nofollow" class="tuijian_auth tuijian_authcolor"> . 李可</a> <span> . 2018</span> </span> </div> </li> </ul> <ul style="display: none;"> <li> <div> <b>1. </b><a class="enjiyixqcontent" href="/patent-detail/06120100421229.html">基于超滤-液相色谱-质谱快速筛选药物活性成分的方法</a> <b>[P]</b> . <span> 中国专利： CN109596749A </span> <span> . 2019-04-09</span> </div> </li> <li> <div> <b>2. </b><a class="enjiyixqcontent" href="/patent-detail/06120106142782.html">液相色谱/串联质谱联用快速筛选和鉴定具有特定结构的化合物</a> <b>[P]</b> . <span> 中国专利： CN101957351A </span> <span> . 2011-01-26</span> </div> </li> <li> <div> <b>3. </b><a class="enjiyixqcontent" href="/patent-detail/06130439097784.html">Screening analysis for unknown substance, especially non-metal automobile components, uses gas or liquid chromatography with mass spectrometry and databases of known retention indexes and mass spectra and substances</a> <b>[P]</b> . <span> 外国专利：  DE10324149A1 </span> <span> . 2004-12-16</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：对未知物质（尤其是非金属汽车部件）进行的筛选分析，采用气相色谱或液相色谱质谱联用，以及已知保留指数，质谱和物质的数据库 </span> </p> </li> <li> <div> <b>4. </b><a class="enjiyixqcontent" href="/patent-detail/06130500096994.html">LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY METHODS FOR THE ANALYSIS OF POLAR MOLECULES</a> <b>[P]</b> . <span> 外国专利：  EP3829733A1 </span> <span> . 2021-06-09</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：液相色谱/质谱法分析极性分子 </span> </p> </li> <li> <div> <b>5. </b><a class="enjiyixqcontent" href="/patent-detail/06130401422997.html">LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY METHODS FOR THE ANALYSIS OF POLAR MOLECULES</a> <b>[P]</b> . <span> 外国专利：  US2020033304A1 </span> <span> . 2020-01-30</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：液相色谱/质谱法分析极性分子 </span> </p> </li> </ul> </div> </div> </div> <div class="theme cardcommon" style="overflow: auto;display:none"> <h3 class="all_title" id="enpatent55">相关主题</h3> <ul id="subject"> </ul> </div> </div> </div> </div> <div class="right rightcon"> <div class="details_img cardcommon clearfix" style="margin-bottom: 10px;display:none;" > </div> </div> </div> <div id="thesis_get_original1" class="downloadBth" 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