Simultaneous analysis by Quadrupole‐Orbitrap mass spectrometry and UHPLC‐MS/MS for the determination of sedative‐hypnotics and sleep inducers in adulterated products

Lee Ji Hyun; Park Han Na; Choi Ji Yeon; Kim Nam Sook; Park Hyung‐Joon; Park Seong Soo; Baek Sun Young

摘要

Abstract >Adulterated products are continuously detected in society and cause problems. In this study, we developed and validated a method for determining synthetic sedative‐hypnotics and sleep inducers, including barbital, benzodiazepam, zolpidem, and first‐generation antihistamines, in adulterated products using Quadrupole‐Orbitrap mass spectrometry and ultrahigh performance liquid chromatography with tandem mass spectrometry. In Quadrupole‐Orbitrap mass spectrometry analysis, target compounds were confirmed using a combination of retention time, mass tolerance, mass accuracy, and fragment ions. For quantification, several validation parameters were employed using ultrahigh performance liquid chromatography with tandem mass spectrometry. The limit of detection and limit of quantitation was 0.05–53 and 0.17–177?ng/mL, respectively. The correlation coefficient for linearity was more than 0.995. The intra‐ and interassay accuracies were 86–110 and 84–111%, respectively. Their precision values were evaluated as within 4.0 (intraday) and 10.7% (interday). Mean recoveries of target compounds in adulterated products ranged from 85 to 116%. The relative standard deviation of stability was less than 10.7% at 4°C for 48?h. The 144 adulterated products obtained over 3 years (2014–2016) from online and in‐person vendors were tested using established methods. After rapidly screening with Quadrupole‐Orbitrap mass spectrometry, the detected samples were quantified using ultrahigh performance liquid chromatography with tandem mass spectrometry. Two of them were adulterated with phenobarbital. </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> >在社会中不断检测到掺假产品并导致问题。在这项研究中，我们开发并验证了使用四轴 - 轨道物质谱和超高性能液相色谱法在掺假产品中测定合成镇静催眠和睡眠诱导剂，包括伴有掺假产品的掺杂产品和串联质量的掺假产品光谱法。在四氢吲哚-β硝基质谱分析中，使用保留时间，质量耐受性，质量准确度和片段离子的组合来确认靶化合物。为了定量，使用具有串联质谱法的超高性能液相色谱法使用几种验证参数。检测极限和定量极限分别为0.05-53和0.17-177Ω·ng / ml。线性的相关系数大于0.995。介入和中间的含量分别为86-110和84-111％。它们的精确值在4.0内（日内）和10.7％（间期）进行评估。掺假产品中靶化合物的平均回收率范围为85至116％。稳定性的相对标准偏差在4℃下小于10.7％，48℃。使用已建立的方法测试从网上和人口供应商中获得3岁以上的144个掺假产品。在用四氧氢吲哚-orbitrap质谱中快速筛选后，使用具有串联质谱法的超高性能液相色谱法定量检测的样品。其中两个掺假苯巴比妥。</ p> </摘要> </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-35800/'>《Journal of separation science. 》</a> <b style="margin: 0 2px;">|</b><span>2017年第24期</span><b style="margin: 0 2px;">|</b> <span>共12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=Lee Ji Hyun&option=202" target="_blank" rel="nofollow">Lee Ji Hyun;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Park Han Na&option=202" target="_blank" rel="nofollow">Park Han Na;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Choi Ji Yeon&option=202" target="_blank" rel="nofollow">Choi Ji Yeon;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Kim Nam Sook&option=202" target="_blank" rel="nofollow">Kim Nam Sook;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Park Hyung‐Joon&option=202" target="_blank" rel="nofollow">Park Hyung‐Joon;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Park Seong Soo&option=202" target="_blank" rel="nofollow">Park Seong Soo;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Baek Sun Young&option=202" target="_blank" rel="nofollow">Baek Sun Young;</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>Division of Advanced Analysis Toxicological Evaluation and Research Department National Institute of Food and Drug Safety EvaluationMinistry of Food and Drug SafetyCheongju‐si Chungcheongbuk‐do Republic of Korea;</p> <p>Division of Advanced Analysis Toxicological Evaluation and Research Department National Institute of Food and Drug Safety EvaluationMinistry of Food and Drug SafetyCheongju‐si Chungcheongbuk‐do Republic of Korea;</p> <p>Division of Advanced Analysis Toxicological Evaluation and Research Department National Institute of Food and Drug Safety EvaluationMinistry of Food and Drug SafetyCheongju‐si Chungcheongbuk‐do Republic of Korea;</p> <p>Division of Advanced Analysis Toxicological Evaluation and Research Department National Institute of Food and Drug Safety EvaluationMinistry of Food and Drug SafetyCheongju‐si Chungcheongbuk‐do Republic of Korea;</p> <p>Division of Advanced Analysis Toxicological Evaluation and Research Department National Institute of Food and Drug Safety EvaluationMinistry of Food and Drug SafetyCheongju‐si Chungcheongbuk‐do Republic of Korea;</p> <p>Division of Advanced Analysis Toxicological Evaluation and Research Department National Institute of Food and Drug Safety EvaluationMinistry of Food and Drug SafetyCheongju‐si Chungcheongbuk‐do Republic of Korea;</p> <p>Division of Advanced Analysis Toxicological Evaluation and Research Department National Institute of Food and Drug Safety EvaluationMinistry of Food and Drug SafetyCheongju‐si Chungcheongbuk‐do Republic of Korea;</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/159.html" title="化学">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=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=liquid chromatography&option=203" rel="nofollow">liquid chromatography;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=sedative‐hypnotics&option=203" rel="nofollow">sedative‐hypnotics;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=sleep inducers&option=203" rel="nofollow">sleep inducers;</a> </p> <div class="translation"> 机译：高分辨率质谱;液相色谱;镇静 - 催眠术;睡眠诱导者; </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/0704025845909.html">Simultaneous analysis by Quadrupole‐Orbitrap mass 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