Abstract
In this paper, we developed an experimental method via LC–MS/MS that enables simultaneous analysis of pymetrozine, ethoxyquin, and cycloxydim, which are pesticide substances used in sweet pepper, and we improved the accuracy of the corresponding experimental method by calculating the uncertainty of measurement. Sweet pepper samples mixed with 5 N sodium hydroxide were extracted with ACN and 1 g of NaCl and 4 g of MgSO4. Verification was conducted using linearity, sensitivity, selectivity, and accuracy. As a result, the limits of detection (LOD) were measured between 2.0 and 3.9 µg/kg, and the limits of quantification (LOQ) were between 6.1 and 11.8 µg/kg. The average recovery rate of the three substances was 97.39–99.42%. The uncertainty of measurement was calculated after identifying various factors that influence the quantitative analysis. The expanded uncertainties of pymetrozine, ethoxyquin, and cycloxydim were 0.47 μg/L, 0.50 μg/L, and 0.49 μg/L, respectively, at a confidence level of approximately 95%. Additionally, k = 2, which was calculated as 4.6%, 5.0%, and 4.6% of the result, respectively. Factors such as the sample weighing, temperature, dilution, and calibration curves were found to affect the uncertainty of measurement. When all the factors were considered, significant results were found, and thus, we judged that this method is suitable for simultaneous analysis of specific residual substances used in sweet pepper.
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Conceptualization: Hyoyoung Kim and Ho Jin Kim; methodology: Hyoyoung Kim; software: Sung Ho Jang; validation: Sung Ho Jang and Han Yeol Bang; data curation: Ho Jin Kim; writing—original draft preparation: Sung Ho Jang and Han Yeol Bang; writing—review and editing: Hyoyoung Kim, Suel Hye Hur, and Eun Joo Baek; project administration: Ho Jin Kim. All authors have read and agreed to the published version of the manuscript.
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Han Yeol Bang declares that he has no conflict of interest. Sung Ho Jang declares that he has no conflict of interest. Eun Joo Baek declares that he has no conflict of interest. Suel Hye Hur declares that he has no conflict of interest. Hyoyoung Kim declares that he has no conflict of interest. Ho Jin Kim declares that he has no conflict of interest.
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Bang, H.Y., Jang, S.H., Baek, E.J. et al. Simultaneous Analysis and Uncertainty of Measurement for Pymetrozine, Ethoxyquin, and Cycloxydim in Sweet Pepper using LC–MS/MS. Food Anal. Methods 16, 1227–1236 (2023). https://doi.org/10.1007/s12161-023-02485-6
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DOI: https://doi.org/10.1007/s12161-023-02485-6