Gas chromatography-mass spectrometric determination of organic acids by ion pair liquid extraction followed by in-situ butylation from aqua feed samples.

IF 16.4 1区化学 Q1 CHEMISTRY, MULTIDISCIPLINARY

Accounts of Chemical Research Pub Date : 2022-02-01 Epub Date: 2022-06-23 DOI:10.1177/14690667221103227

Kalpana Talari, Sai Krishna Ganji, Satish Mutyam, Raja Rajeswari Tiruveedula

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引用次数: 1

Abstract

A rapid and sensitive analytical method was developed to quantitatively determine organic acids (OAs) from fish feed samples extracted by ion-pair (IP) solvent extraction, followed by in-situ butylation and gas chromatography-mass spectrometric (GC-MS) analysis. The extraction of OAs was carried out with acetonitrile containing 10 mM tetrabutylammonium hydroxide (TBAH), and the analytes were derivatized to their butyl esters in the injection port of the GC-MS system. The developed method was validated in the range of 1-5000 ng/g, with recoveries ranging from 93-117%. The limit of detection (LOD) and limit of quantification (LOQ) of the method was 1-5 ng/g and 2-10 ng/g, respectively, yielding good linearity (R² > 0.9990) and precision with a relative standard deviation less than 10%. The proposed method was successfully applied to analyze OAs in sinking and floating fish feed samples. The analyzed samples showed the presence of benzoic, succinic, fumaric, glutaric, adipic, and phthalic acids in sinking feed samples; and benzoic, succinic, adipic, phthalic acids in floating feed samples, respectively.

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气相色谱-质谱联用离子对液体萃取-原位丁化法测定水产饲料样品中的有机酸。

采用离子对(IP)溶剂萃取、原位丁基化、气相色谱-质谱联用(GC-MS)技术，建立了一种快速、灵敏的测定鱼饲料中有机酸含量的方法。用含有10 mM四丁基氢氧化铵(TBAH)的乙腈进行萃取，在气相色谱-质谱联用系统的进样口将分析物衍生为相应的丁酯。该方法在1 ~ 5000 ng/g范围内有效，回收率为93 ~ 117%。方法的检出限和定量限分别为1 ~ 5 ng/g和2 ~ 10 ng/g，线性良好(R2 > 0.9990)，精密度相对标准偏差小于10%。该方法已成功应用于沉鱼和浮鱼饲料样品中oa的分析。沉饲料样品中存在苯甲酸、琥珀酸、富马酸、戊二酸、己二酸和邻苯二甲酸;以及浮游饲料样品中的苯甲酸、琥珀酸、己二酸、邻苯二甲酸。

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来源期刊

Accounts of Chemical Research 化学-化学综合

CiteScore

31.40

自引率

1.10%

发文量

312

审稿时长

2 months

期刊介绍： Accounts of Chemical Research presents short, concise and critical articles offering easy-to-read overviews of basic research and applications in all areas of chemistry and biochemistry. These short reviews focus on research from the author’s own laboratory and are designed to teach the reader about a research project. In addition, Accounts of Chemical Research publishes commentaries that give an informed opinion on a current research problem. Special Issues online are devoted to a single topic of unusual activity and significance. Accounts of Chemical Research replaces the traditional article abstract with an article "Conspectus." These entries synopsize the research affording the reader a closer look at the content and significance of an article. Through this provision of a more detailed description of the article contents, the Conspectus enhances the article's discoverability by search engines and the exposure for the research.