Analytical Validation of a Reversed-Phase Ion Pairing HPLC-DAD Method for the Simultaneous Determination of Anthropogenic Pollutants

IF 0.7 Q4 CHEMISTRY, ANALYTICAL Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI:10.17721/moca.2023.13-21
Liew Sook Ling, Ivan Kok Seng Yap, Chong Chun Wie, Wong Lai Chun
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Abstract

Caffeine, trigonelline, nicotinamide, and hippuric acid are potential organic markers of anthropogenic activities in the environment. In this work, a selective, precise, accurate, and robust reverse phase high performance liquid chromatography with a diode array detection method was developed for their simultaneous determination. Chromatographic analysis was achieved on GraceSmart RP C18 (150 mm x 4.6 mm, 5 μm) column. The mobile phase was 20 mM ammonium acetate buffer (pH 4.5) and methanol in gradient elution mode at a flow rate of 1.0 mL min-1, with 5 mM heptafluorobutyric acid as an ion pairing agent. Detection was performed at 275 nm for caffeine, 265 nm for trigonelline, 261 nm for nicotinamide, and 250 nm for hippuric acid. The method was validated as per the International Conference on Harmonization guidelines. Linear responses were found in the concentration range of 10-200 μg mL-1 with a correlation coefficient of at least 0.999. The percent relative standard deviation of intra-day precision, inter-day precision, and robustness was less than 2 %. The accuracy, expressed as percentage recovery ranged between 93.23 – 99.22%. Values for limits of detection and quantification were between 0.07-0.34 μg mL-1, and 0.21-1.04 μg mL-1, respectively. Lake samples from public parks were collected and subjected to analysis using the validated method
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反相离子配对HPLC-DAD法同时测定人为污染物的分析验证
咖啡因、葫芦巴碱、烟酰胺和马尿酸是环境中人类活动的潜在有机标志物。本研究建立了一种选择性、精密度、准确度和鲁棒性强的反相高效液相色谱二极管阵列检测方法。色谱分析采用GraceSmart RP C18 (150 mm x 4.6 mm, 5 μm)色谱柱。流动相为20 mM醋酸铵缓冲液(pH为4.5)和甲醇,梯度洗脱,流速为1.0 mL min-1, 5 mM七氟丁酸为离子配对剂。咖啡因的检测波长为275 nm,葫芦巴碱为265 nm,烟酰胺为261 nm,马尿酸为250 nm。该方法按照国际协调会议的准则进行了验证。在10 ~ 200 μ mL-1浓度范围内呈线性关系,相关系数至少为0.999。日内精密度、日内精密度和稳健性的相对标准偏差百分比小于2%。准确度在93.23 ~ 99.22%之间,以回收率表示。检出限为0.07 ~ 0.34 μ mL-1,定量限为0.21 ~ 1.04 μ mL-1。采集公园湖泊样本,采用验证方法进行分析
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来源期刊
CiteScore
1.00
自引率
14.30%
发文量
12
期刊介绍: The journal "Methods and objects of chemical analysis" is peer-review journal and publishes original articles of theoretical and experimental analysis on topical issues and bio-analytical chemistry, chemical and pharmaceutical analysis, as well as chemical metrology. Submitted works shall cover the results of completed studies and shall make scientific contributions to the relevant area of expertise. The journal publishes review articles, research articles and articles related to latest developments of analytical instrumentations.
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