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| Nonderivatized Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Histamine in Fish Meat |
| ZHANG Xiaomin, XIAO Jingcheng, XIAO Hongtao, WANG Sheng, SUN Rong, ZHANG Di, LI Shenghua, YANG Chunyan |
| 1. College of Public Health, Inner Mongolia Medical University, Hohhot 010059, China; 2. Erdos City Center for Disease Control and Prevention, Erdos 017010, China |
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Abstract In this study, a liquid chromatography-tandem mass spectrometry (MS/MS) method was developed for the detection of histamine in fish. A 70:20:10 (V/V) mixture of methanol, acetonitrile and water containing 0.2% (V/V) formic acid was used as the extraction solvent. Lipids, proteins, and other impurities in fish samples were removed by liquid nitrogen freezing followed by centrifugation. Chromatographic separation was performed on a Diol-HILIC-120 column (2.1 mm × 100 mm, 1.9 μm) using gradient elution. The mobile phase consisted of 0.5% (V/V) formic acid solution (containing 10 mmol/L ammonium formate) and 90% (V/V) acetonitrile solution (containing 10 mmol/L ammonium formate and 0.5% (V/V) formic acid). Detection was carried out using electrospray ionization in the positive mode. The results showed that the calibration curve for histamine exhibited good linearity in the concentration range of 2–250 μg/L, with a correlation coefficient (R2) of 0.999 98. The limits of detection and quantitation were 0.5 and 1.6 μg/kg, respectively. The recovery rates for spiked samples ranged from 84.36% to 109.43%, with relative standard deviations (RSDs) below 5%. This method was used to detect 20 fish samples from 10 species sold in the market, showing that the detection rate was 95% and histamine levels in all samples were below the limit stipulated by the Chinese national standard. The proposed method is simple and highly sensitive, and enables rapid detection of histamine in fish, providing efficient and environmentally friendly technical support for the detection of histamine in fish and other aquatic products.
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2026, Vol. 40 
