A Sensitive Liquid Chromatography-Mass Spectrometric Method for Determination of Bisoprolol in Rat Serum after Pre-Column Derivatization.

IF 1.5 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS Journal of chromatographic science Pub Date : 2024-08-20 DOI:10.1093/chromsci/bmad056

Huda A Shaheen, Saleh O Bahaffi, Alaa M Khedr

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Abstract

Two derivatization regents were reacted with bisoprolol (BIS), followed by liquid-chromatography-mass spectrometric analysis. 3-Bromomethyl-propyphenazone (BMP) and dansyl-chloride (Dns-Cl) were reacted via the secondary amino group using a catalyst to accelerate the reaction progress and completeness with minimal reaction byproducts. The sensitivity and the ionization efficiency of both BIS-methyl-propyphenazone (BIS-MP) and BIS-Dns via electrospray ionization were studied. The sensitivity of BIS-MP was superior to BIS-Dns. The derivatization procedure, extraction procedure, and LC-MS method were optimized and validated to achieve the monitoring of BIS in rat serum at a picogram scale. The calibration curve showed a regression coefficient value of 0.999 within a concentration spanning a range of 10-500 pg/mL. The detection limit and quantitation were 4 and 10 pg/mL, respectively. The intraday and inter-day precision values (% relative standard deviation) ranged from 0.53 to 6.91%, whereas the accuracy values (expressed as % error) ranged from -4.20 to -0.77%. The pharmacokinetic parameters were: 15,280 pg/mL for a maximum concentration of BIS (Cmax) at the maximum time (Tmax) of 1 h. BIS's elimination half-life (t1/2) was determined to be 3 h. The value of the area under the concentration-time curve (AUC0 - t) was 34,370 pg/mL h.

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柱前衍生化后测定大鼠血清中比索洛尔的灵敏液相色谱-质谱法

两种衍生调节剂与比索洛尔（BIS）反应，然后进行液相色谱-质谱分析。3-Bromomethyl-propyphenazone (BMP) 和 dansyl-chloride (Dns-Cl) 通过仲氨基进行反应，使用催化剂可加快反应的进程和完整性，并将反应副产物降至最低。通过电喷雾离子化技术研究了 BIS-甲基-丙基哒嗪（BIS-MP）和 BIS-Dns 的灵敏度和离子化效率。BIS-MP 的灵敏度优于 BIS-Dns。对衍生化步骤、萃取步骤和 LC-MS 方法进行了优化和验证，以实现对大鼠血清中 BIS 的皮克级监测。在 10-500 pg/mL 的浓度范围内，校正曲线的回归系数为 0.999。检测限和定量分别为 4 和 10 pg/mL。日内和日间精密度值（相对标准偏差百分比）在 0.53% 至 6.91% 之间，而准确度值（以误差百分比表示）在 -4.20% 至 -0.77% 之间。药代动力学参数为BIS 的消除半衰期（t1/2）被确定为 3 小时。浓度-时间曲线下面积（AUC0 - t）的值为 34,370 pg/mL h。

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来源期刊

Journal of chromatographic science 化学-分析化学

CiteScore

2.90

自引率

7.70%

发文量

审稿时长

5.6 months

期刊介绍： The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.