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Optimization and Validation of a Method for Analysis of Non-Volatile Organic Acids in Baijiu by Derivatization and its Application in Three Flavor-Types of Baijiu

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Abstract

Organic acids have essential effects on the flavor of Baijiu. Except for some small molecular organic acids, which are volatile, most of other organic acids are non-volatile. And due to their low contents in Baijiu, the detection of non-volatile organic acids (NVOAs) in Baijiu is a challenging work. In this study, an optimized derivatization method was developed to detect the NVOAs in Baijiu. Optimization on the derivatization reagent, reaction time and temperature revealed that 10 mL of Baijiu was concentrated to dryness, followed by adding 100 μL BSTFA and 50 μL pyridine and subsequent derivatization over 3 h at 80 °C was suitable. Under the optimal conditions, excellent linearity for all NVOAs was obtained with determination coefficients of R2 > 0.99, inter-day and intra-day precision were below 7.30% and 6.90%, respectively, and recovery rates were in the range of 80.64–113.46%. The LODs were between 0.05 and 11.75 μg/L, which were one-fifth to one ten-thousandth of those detected by HPLC and HPLC–MS. Thirty-six NVOAs in soy sauce (SS), strong (ST), and Laobaigan (LBG) flavor-types of Baijiu were identified. The concentration of lactic acid among the three types of Baijiu was the highest, whose contents were (1069.16 ± 58.74, 7330.11 ± 47.67, 2054.02 ± 54.15) mg/L in LBG, SS, and ST, respectively. Besides, the NVOAs in these three Baijiu were quite different according to principal component analysis and hierarchical cluster analysis. This study provides an effective method for the analysis of NVOAs in complex matrix foods.

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Funding

This work was supported by the National Key R&D Program of China [2016YFD0400500] and the National Natural Science Foundation of China [32001826].

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Guangnan Wang: investigation and writing-original draft. Xing Li: data curation and investigation. Xuebo Song: investigation and software. Si Jing: investigation and software. Shihao Meng: software. Fuping Zheng: research scheme design and supervision. Hehe Li: software. Zexia Li: supervision. Caihong Shen: supervision. Yi Shen: supervision.

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Correspondence to Fuping Zheng.

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Guangnan Wang declares that he/she has no Conflict of interest. Xing Li declares that he/she has no Conflict of interest. Xuebo Song declares that he/she has no Conflict of interest. Si Jing declares that he/she has no Conflict of interest. Shihao Meng declares that he/she has no Conflict of interest. Fuping Zheng declares that he/she has no Conflict of interest. Hehe Li declares that he/she has no Conflict of interest. Zexia Li declares that he/she has no Conflict of interest. Caihong Shen declares that he/she has no Conflict of interest. Yi Shen declares that he/she has no Conflict of interest.

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Wang, G., Li, X., Song, X. et al. Optimization and Validation of a Method for Analysis of Non-Volatile Organic Acids in Baijiu by Derivatization and its Application in Three Flavor-Types of Baijiu. Food Anal. Methods 15, 1606–1618 (2022). https://doi.org/10.1007/s12161-021-02215-w

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  • DOI: https://doi.org/10.1007/s12161-021-02215-w

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