Determination of Sixteen Kinds of Free Amino Acids in Citrus by Liquid Liquid Microextraction/Solid Phase Microextraction Coupled with Gas Chromatography

WANG Yulong; LI Xiaoqing; LI Xiujuan

doi:10.13386/j.issn1002-0306.2022080304

Volume 44 Issue 12

Jun. 2023

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Science and Technology of Food Industry > 2023 > 44(12): 285-292. > DOI: 10.13386/j.issn1002-0306.2022080304

WANG Yulong, LI Xiaoqing, LI Xiujuan. Determination of Sixteen Kinds of Free Amino Acids in Citrus by Liquid Liquid Microextraction/Solid Phase Microextraction Coupled with Gas Chromatography[J]. Science and Technology of Food Industry, 2023, 44(12): 285−292. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022080304.

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Determination of Sixteen Kinds of Free Amino Acids in Citrus by Liquid Liquid Microextraction/Solid Phase Microextraction Coupled with Gas Chromatography

1.
College of Pharmacopolist, Zhejiang Pharmaceutical University, Ningbo 315500, China
2.
Jining Academy of Agricultural Sciences, Jining 272000, China
3.
College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, China

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Received Date: August 30, 2022
Available Online: April 10, 2023

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Abstract

Abstract

Objective: To evaluate the quality of the citrus, a gas chromatography (GC) coupled with flame ion detector was established for the determination of sixteen kinds of free amino acids in citrus simultaneously. Methods: Firstly, the single factor tests werre used to optimize the derivatization conditions of isobutyl chloroformate. Subsequently, a method was developed by liquid-liquid microextraction (LLME)/solid phase microextraction (SPME) coupled with GC using a home-made sol-gel butylmethacrylate/divinylbenzene (BMA/DVB) fibers. Results: The results showed that the derivatization conditions were the best under one derivation with one min. The best SPME conditions can be obtained as follows: The extraction temperature of 40 ℃, the extraction time of 30 min and the 30% sodium sulfate at the extraction speed of 1000 r·min⁻¹. Under the optimized experimental parameters, there were good linear relationships for 16 analytes with correlation coefficients larger than 0.99. The limit of detection was 0.85~12.60 μg·kg⁻¹ and the standard recoveries of the spiked samples ranged from 82.51% to 121.75%, with relative standard deviations of 2.51%~12.80%. Conclusion: The method was convenient, accurate, and matrix resistant. It could be used as a new model for the determination of the free amino acids in citrus pulp samples and can also provide a valuable reference for the quality evaluation of cirtrus.
- citrus,
- free amino acids,
- liquid-liquid microextraction (LLME),
- solid phase microextraction (SPME),
- gas chromatography (GC)

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