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采用设计质量分析法测定环境水样中硝酸盐和亚硝酸盐含量的新型、快速、简便等度超高效液相色谱-紫外检测法

Novel, Rapid, and Simple Isocratic UPLC-UV Method for Estimating Nitrate and Nitrite Contents in Environmental Water Samples Using an Analytical Quality by Design Approach.

作者信息

Gollapudi Pradeep Kumar, Gollapudi Kranthi Kumar, Padmaja Dr Nimmagadda

机构信息

Dr Reddy's Laboratories, IPDO, API AR&D Bachupally, Hyderabad 500090, India.

Professor, Department of Chemistry, ANITS College, Visakhapatnam 531162, India.

出版信息

ACS Omega. 2024 Dec 12;9(51):50504-50514. doi: 10.1021/acsomega.4c07912. eCollection 2024 Dec 24.

DOI:10.1021/acsomega.4c07912
PMID:39741822
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11683632/
Abstract

In this study, we reported a novel reverse-phase UPLC method for the simultaneous estimation of nitrite and nitrate ions using a Quality by Design (QbD) approach. Nitrite and nitrate ions were separated on an ACQUITY CSH Fluoro-Phenyl column (100 × 2.1 mm, 1.7 μm) in isocratic mode with a mobile phase composition of solvent A and solvent B in a ratio of 980:20 v/v. Solvent A consisted of 100% Milli-Q water, while solvent B comprised 0.5 mL of formic acid in 1000 mL of methanol. The column temperature was maintained at 40 °C, and the flow rate was 0.6 mL/min. Detection was carried out at 214 nm with an injection volume of 5.0 μL. The method was developed and validated in accordance with ICH Q2 (R2) guidelines Validation parameters, including system suitability, sensitivity, precision, linearity, and accuracy, were within acceptable ranges. These findings suggest that the developed RP-UPLC method is highly sensitive and suitable for the estimation of nitrite and nitrate ions in various environmental water samples.

摘要

在本研究中，我们报告了一种采用质量源于设计（QbD）方法同时测定亚硝酸根离子和硝酸根离子的新型反相超高效液相色谱（UPLC）方法。亚硝酸根离子和硝酸根离子在ACQUITY CSH氟苯基色谱柱（100×2.1 mm，1.7μm）上采用等度模式分离，流动相由溶剂A和溶剂B按980:20 v/v的比例组成。溶剂A由100%超纯水组成，而溶剂B由1000 mL甲醇中加入0.5 mL甲酸组成。柱温保持在40℃，流速为0.6 mL/min。检测波长为214 nm，进样体积为5.0μL。该方法按照国际人用药品注册技术协调会（ICH）Q2（R2）指南进行开发和验证。包括系统适用性、灵敏度、精密度、线性和准确度在内的验证参数均在可接受范围内。这些结果表明，所开发的反相超高效液相色谱方法具有高灵敏度，适用于各种环境水样中亚硝酸根离子和硝酸根离子的测定。

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本文引用的文献

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Determining Nitrate and Nitrite Content in Beverages, Fruits, Vegetables, and Stews Marketed in Arak, Iran.测定伊朗阿拉克市市场上销售的饮料、水果、蔬菜和炖菜中的硝酸盐和亚硝酸盐含量。
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