Determination of sodium cromoglycate in human plasma by liquid chromatography–mass spectrometry in the turbo ion spray mode

M.L Ozoux , J Girault , J.M Malgouyat , O Pasquier
{"title":"Determination of sodium cromoglycate in human plasma by liquid chromatography–mass spectrometry in the turbo ion spray mode","authors":"M.L Ozoux ,&nbsp;J Girault ,&nbsp;J.M Malgouyat ,&nbsp;O Pasquier","doi":"10.1016/S0378-4347(01)00420-0","DOIUrl":null,"url":null,"abstract":"<div><p>A highly sensitivity liquid chromatography–tandem mass spectrometry method has been developed for the quantitation of sodium cromoglycate (SCG) in human plasma. The method was validated over a linear range of 0.100–50.0 ng/ml, using <sup>13</sup>C<sub>4</sub> sodium cromoglycate as the internal standard. Compounds were extracted from 1.0 ml of lithium heparin plasma by methanol elution of C<sub>18</sub> solid-phase extraction cartridges. The dried residue was reconstituted with 100 μl of 0.01 N HCl, and 30 μl was injected onto the LC–MS–MS system. Chromatographic separation was achieved on a C8 (3.5 μm) column with an isocratic mobile phase of methanol–water–0.5 <em>M</em> ammonium acetate (35:64.8:0.2, v/v/v). The analytes were detected with a PE Sciex API 3000 mass spectrometer using turbo ion spray with positive ionization. Ions monitored in the multiple reaction monitoring (MRM) mode were <em>m</em>/<em>z</em> 469.2 (precursor ion) to <em>m</em>/<em>z</em> 245.1 (product ion) for SCG and <em>m</em>/<em>z</em> 473.2 (precursor ion) to <em>m</em>/<em>z</em> 247.1 (product ion) for <sup>13</sup>C<sub>4</sub> SCG (I.S.). The average recoveries of SCG and the I.S. from human plasma were 91 and 87%, respectively. The low limit of quantitation was 0.100 ng/ml. Results from a 4-day validation study demonstrated excellent precision (C.V.% values were between 1.9 and 6.5%) and accuracy (−5.4 to −1.2%) across the calibration range of 0.100–50.0 ng/ml.</p></div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"765 2","pages":"Pages 179-185"},"PeriodicalIF":0.0000,"publicationDate":"2001-12-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00420-0","citationCount":"24","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chromatography B: Biomedical Sciences and Applications","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0378434701004200","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 24

Abstract

A highly sensitivity liquid chromatography–tandem mass spectrometry method has been developed for the quantitation of sodium cromoglycate (SCG) in human plasma. The method was validated over a linear range of 0.100–50.0 ng/ml, using 13C4 sodium cromoglycate as the internal standard. Compounds were extracted from 1.0 ml of lithium heparin plasma by methanol elution of C18 solid-phase extraction cartridges. The dried residue was reconstituted with 100 μl of 0.01 N HCl, and 30 μl was injected onto the LC–MS–MS system. Chromatographic separation was achieved on a C8 (3.5 μm) column with an isocratic mobile phase of methanol–water–0.5 M ammonium acetate (35:64.8:0.2, v/v/v). The analytes were detected with a PE Sciex API 3000 mass spectrometer using turbo ion spray with positive ionization. Ions monitored in the multiple reaction monitoring (MRM) mode were m/z 469.2 (precursor ion) to m/z 245.1 (product ion) for SCG and m/z 473.2 (precursor ion) to m/z 247.1 (product ion) for 13C4 SCG (I.S.). The average recoveries of SCG and the I.S. from human plasma were 91 and 87%, respectively. The low limit of quantitation was 0.100 ng/ml. Results from a 4-day validation study demonstrated excellent precision (C.V.% values were between 1.9 and 6.5%) and accuracy (−5.4 to −1.2%) across the calibration range of 0.100–50.0 ng/ml.

涡流喷雾液相色谱-质谱法测定人血浆中氨基甘氨酸钠
建立了一种高灵敏度液相色谱-串联质谱法定量测定人血浆中甘露糖酸钠的方法。以13C4异甘氨酸钠为内标,在0.100 ~ 50.0 ng/ml的线性范围内验证。从1.0 ml肝素锂血浆中提取化合物,用C18固相萃取筒甲醇洗脱。用100 μl的0.01 N HCl重组干燥后的残渣,并将30 μl注入LC-MS-MS系统。色谱柱为C8 (3.5 μm),流动相为甲醇-水- 0.5 M醋酸铵(35:64.8:0.2,v/v/v)。采用PE Sciex API 3000质谱仪,采用正离子化涡轮喷雾对分析物进行检测。多反应监测(MRM)模式下,SCG监测的离子为m/z 469.2(前体离子)~ m/z 245.1(产物离子),13C4 SCG监测的离子为m/z 473.2(前体离子)~ m/z 247.1(产物离子)。人血浆中SCG和is的平均回收率分别为91%和87%。定量下限为0.100 ng/ml。为期4天的验证研究结果显示,在0.100-50.0 ng/ml的校准范围内,具有优异的精密度(C.V.%值在1.9 - 6.5%之间)和准确度(- 5.4 - - 1.2%)。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
求助全文
约1分钟内获得全文 求助全文
来源期刊
自引率
0.00%
发文量
0
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术官方微信