Development and validation of HPLC-UV and LC-MS/MS methods for the quantitative determination of a novel aminothiazole in preclinical samples

IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY BMC Chemistry Pub Date : 2024-11-07 DOI:10.1186/s13065-024-01321-0
Vinay N. Basavanakatti, Mohammad Ali, D.R. Bharathi, Sheikh Murtuja, Barij Nayan Sinha, Venkatesan Jayaprakash, Faiyaz Shakeel
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Abstract

Aminothiazoles are the important class of chemical groups which have proven their broad range of biological activities. A novel aminothiazole (21MAT) was quantified in analytical solutions using a high-performance liquid chromatography (HPLC) approach that was developed and partially validated for the analysis of in vitro experimental samples. An isocratic elution on reverse phase Phenomenex® Luna C18 (50 mm × 4.6 mm, 5 μm) column with 55% 0.1% v/v orthophosphoric acid in water and 45% of orthophosphoric acid in acetonitrile at a flow rate of 1 mL/min was used. The analyte was detected at 272 nm. Similar to this, a robust bioanalytical technique, LC-mass spectrometry (LC-MS/MS) was created and verified to measure 21MAT in rat plasma for use in in vitro screening study samples and early-stage pharmacokinetic research. The protein precipitation method was used to extract 21MAT from plasma. The mixture of 95: 5% v/v methanol: acetonitrile and 0.1% v/v formic acid, along with 15% of 5 mM ammonium formate solution, was used to separate the mixture on a reverse phase Waters Xterra RP® C18 (150 mm × 4.6 mm, 5 μm) column at a flow rate of 1 mL/min. Using electro spray ionisation mode in multiple reaction monitoring mode, the analyte and internal standard (a structural analogue) were both identified. According to current criteria, all validation parameters (specificity, selectivity, accuracy, precision, recovery, matrix factor, hemolysis effect, and stability) were evaluated in rat plasma. The area response of 21MAT was found to be linear over the concentration range of 1.25–1250 ng/mL in rat plasma. Both techniques are suitable for use in any format of preclinical research and were sufficiently reliable to measure 21MAT precisely in various matrices. In silico prediction helped in understanding absorption, distribution, metabolism, excretion, and toxicity (ADMET) behaviour of the molecule. Both developed LC-MS/MS and HPLC-UV methods were successfully used to quantify the analyte in in vitro screening study samples.

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开发并验证用于定量测定临床前样品中一种新型氨基噻唑的 HPLC-UV 和 LC-MS/MS 方法
氨基噻唑是一类重要的化学物质,已被证明具有广泛的生物活性。本研究采用高效液相色谱法(HPLC)对分析溶液中的一种新型氨基噻唑(21MAT)进行了定量分析。采用反相 Phenomenex® Luna C18(50 mm × 4.6 mm,5 μm)色谱柱,以 55% 0.1% v/v 原磷酸水溶液和 45% 原磷酸乙腈水溶液进行等度洗脱,流速为 1 mL/min。在 272 纳米波长处检测分析物。与此类似,我们还创建并验证了一种稳健的生物分析技术--液相色谱-质谱法(LC-MS/MS),用于测量大鼠血浆中的 21MAT 含量,以用于体外筛选研究样本和早期药代动力学研究。采用蛋白质沉淀法从血浆中提取 21MAT。使用 95% v/v 甲醇:5% v/v 乙腈和 0.1% v/v 甲酸的混合溶液以及 15% 5 mM 甲酸铵溶液,在反相 Waters Xterra RP® C18(150 mm × 4.6 mm,5 μm)色谱柱上分离混合物,流速为 1 mL/min。在多反应监测模式下使用电喷雾离子化模式,对分析物和内标物(一种结构类似物)进行了鉴定。根据现行标准,在大鼠血浆中对所有验证参数(特异性、选择性、准确性、精密度、回收率、基质因子、溶血效应和稳定性)进行了评估。在大鼠血浆中 1.25-1250 纳克/毫升的浓度范围内,21MAT 的面积响应呈线性关系。这两种技术都适用于任何形式的临床前研究,而且在各种基质中精确测量 21MAT 都足够可靠。硅学预测有助于了解该分子的吸收、分布、代谢、排泄和毒性(ADMET)行为。所开发的 LC-MS/MS 和 HPLC-UV 方法均成功用于体外筛选研究样品中分析物的定量。
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来源期刊
BMC Chemistry
BMC Chemistry Chemistry-General Chemistry
CiteScore
5.30
自引率
2.20%
发文量
92
审稿时长
27 weeks
期刊介绍: BMC Chemistry, formerly known as Chemistry Central Journal, is now part of the BMC series journals family. Chemistry Central Journal has served the chemistry community as a trusted open access resource for more than 10 years – and we are delighted to announce the next step on its journey. In January 2019 the journal has been renamed BMC Chemistry and now strengthens the BMC series footprint in the physical sciences by publishing quality articles and by pushing the boundaries of open chemistry.
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