在线固相萃取-液相色谱-串联质谱法测定血清样品中的沙库比特利和七种沙坦类药物

IF 3.1 3区 医学 Q2 CHEMISTRY, ANALYTICAL Journal of pharmaceutical and biomedical analysis Pub Date : 2024-11-22 DOI:10.1016/j.jpba.2024.116580
Yanan Guo , Shuang Cao , Bin Geng , Juanjuan Ma , Bo Yao
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引用次数: 0

摘要

本研究建立了一种在线固相萃取-超高效液相色谱-串联质谱检测方法,用于同时测定血清中的沙库比妥和七种沙坦类药物。化合物经 C18 色谱柱分离。使用喷射流电喷雾离子源(AJS,ESI+)对样品进行质谱分析。样品通过多反应监测(MRM)模式进行检测,并通过稳定同位素内标法进行定量。该方法的进样量为 900 μL,运行时间为 12.5 分钟。8 种目标化合物在相应的质量浓度范围内线性关系良好(r2>0.994),定量下限为 0.05-0.1 μg/L。加标血清样品的回收率为 90.90 % 至 106.20 %,相对标准偏差为 4.57 % 至 9.27 %。使用该方法在实际血清样品中检测到了五种目标化合物。该方法简便、灵敏、准确,适用于血清样品中萨库比特利和7种沙坦类药物的痕量检测。该方法可满足临床监测该类药物血药浓度的需要,同时为萨库比特利和其他沙坦类药物复方制剂的开发提供了检测技术支持。
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Determination of sacubitril and seven sartan drugs in serum samples by online solid phase extraction-liquid chromatography-tandem mass spectrometry
An online solid phase extraction–ultra performance liquid chromatography–tandem mass spectrometry detection method was developed for the simultaneous determination of sacubitril and seven sartan drugs in blood serum in this study. The compounds were separated through a C18 column. Mass spectrometry of the samples was performed using a jet stream electrospray ion source (AJS, ESI+). The samples were detected via a multiple reaction monitoring (MRM) mode and quantified via a stable isotope internal standard method. 900 μL of prepared sample was injected and a run time of 12.5 minutes was obtained in this proposed method. The eight examined target compounds showed good linearity (r2>0.994) in the corresponding mass concentration range and a lower limit of quantitation (LLOQ) was in the range of 0.05–0.1 μg/L. The recovery of the spiked serum samples ranged from 90.90 % to 106.20 % with relative standard deviations (RSDs) of 4.57 %–9.27 %. Five target compounds were detected in the actual serum samples using this method. The proposed method is simple to use, sensitive, accurate, and suitable for the trace detection of sacubitril and seven sartan drugs present in serum samples. The method can meet the needs for clinical monitoring of blood concentrations of this type of drug, while providing detection technology support for the development of compound preparations of sacubitril and other sartan drugs.
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来源期刊
CiteScore
6.70
自引率
5.90%
发文量
588
审稿时长
37 days
期刊介绍: This journal is an international medium directed towards the needs of academic, clinical, government and industrial analysis by publishing original research reports and critical reviews on pharmaceutical and biomedical analysis. It covers the interdisciplinary aspects of analysis in the pharmaceutical, biomedical and clinical sciences, including developments in analytical methodology, instrumentation, computation and interpretation. Submissions on novel applications focusing on drug purity and stability studies, pharmacokinetics, therapeutic monitoring, metabolic profiling; drug-related aspects of analytical biochemistry and forensic toxicology; quality assurance in the pharmaceutical industry are also welcome. Studies from areas of well established and poorly selective methods, such as UV-VIS spectrophotometry (including derivative and multi-wavelength measurements), basic electroanalytical (potentiometric, polarographic and voltammetric) methods, fluorimetry, flow-injection analysis, etc. are accepted for publication in exceptional cases only, if a unique and substantial advantage over presently known systems is demonstrated. The same applies to the assay of simple drug formulations by any kind of methods and the determination of drugs in biological samples based merely on spiked samples. Drug purity/stability studies should contain information on the structure elucidation of the impurities/degradants.
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