Determination of Sex Hormone Residues in Shrimp by EMR Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

XIN Lina; MO Dongshu; JIANG Dingzhi; ZENG Jian; LIANG Feiyan; MENG Chuxi

doi:10.13386/j.issn1002-0306.2021040071

Volume 43 Issue 2

Jan. 2022

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Science and Technology of Food Industry > 2022 > 43(2): 263-270. > DOI: 10.13386/j.issn1002-0306.2021040071

XIN Lina, MO Dongshu, JIANG Dingzhi, et al. Determination of Sex Hormone Residues in Shrimp by EMR Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2022, 43(2): 263−270. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021040071.

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Determination of Sex Hormone Residues in Shrimp by EMR Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Guangxi-Asean Food and Drug Safety Inspection and Testing Center, Nanning 530021, China

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Received Date: April 08, 2021
Available Online: November 15, 2021

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Abstract

Abstract

A method for the determination of 15 sex hormones in shrimp meat by EMR solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry was established. The samples was extracted with 0.1 mol/L ethylenediaminetetraacetic acid disodium solution and acetonitrile solution, purified by Captiva EMR SPE cartridge, separated by CAPCELLPAK C₁₈ BB-H (3 µm, 2.1 mm×150 mm) column, and scanned by positive and negative ions of electrospray ion source. Ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with multiple reaction monitoring mode was used for detection, and blank matrix matching external standard method was used for quantification. The positive ion mobile phase was methanol and 0.1% formic acid, and androgen and progesterone were detected. The negative ion mobile phase was acetonitrile and 0.01% ammonia aqueous solution to detect estrogen. The results showed that the 15 kinds of sex hormone residues in shrimp meat samples purified by EMR solid phase extraction had a good linear relationship in the concentration range of 1~50 μg/kg, and the correlation coefficients (r) were all greater than 0.99. The detection limits of the method were 0.0015~0.436 μg/kg, and the quantitative limits were 0.0051~1.453 μg/kg. The average recoveries were 85.31%~119.84%, and the relative standard deviations were 2.11%~9.86% (n=6). The method was rapid, simple, reproducible and sensitive, which was suitable for the detection of 15 kinds of sex hormone residues in shrimp meat.

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