Establishing a method of HPLC involving precolumn derivatization by 2,2'-dithiobis (5-nitropyridine) to determine the sulfites in shrimps in comparison with ion chromatography

建立一种采用2,2'-二硫代双(5-硝基吡啶)进行柱前衍生化的高效液相色谱法测定虾中亚硫酸盐含量,并与离子色谱法进行比较。

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Abstract

Although sulfites are widely used in shrimp processing, the contents of residual sulfite need to be strictly controlled due to their potential toxicity. In this paper, a novel method was developed for determination of the free and total sulfites in shrimps. Major procedures of the method includes separation of free and total sulfites with ultrasound-assisted extraction and pH adjustment for 20 min, then a precolumn derivatization was conducted by 2,2'-Dithiobis (5-nitropyridine) and verified by LC-MS, and finally HPLC coupled with an ultraviolet (UV) detector was carried out. Results indicated that the UV absorption wavelength shifted from 213 (sulfites) to 320 nm (new disulfide compounds), significantly reducing the interference of natural occurring compounds and solvents in the matrix. The standard curves exhibited a good linear range of 3.2-51.2 mg/L (R (2) = 0.9996). The limit of detection (LOD) and limit of quantification (LOQ) were 0.3 and 1.0 mg/L, respectively. The contents of free and total sulfite in frozen shrimps were 26.58 ± 0.48 and 31.44 ± 0.83 mg/kg calculated by SO(2), respectively. These were similar (p > 0.05) to the data obtained by the method of ion chromatography. In conclusion, the new developed method has been proved to be a reliable and economic method for effective determination of free and total sulfites in the shrimps, and the method could be expanded in determination of the sulfites in other food products.

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