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标题：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
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作者：Kai Yang ; Cheng Zhou ; Zhenhuan Yang 等
期刊名称：Food Science & Nutrition
电子版ISSN：2048-7177
出版年度：2019
卷号：7
期号：6
页码：2151-2158
DOI：10.1002/fsn3.1060
出版社：John Wiley & Sons, Ltd.
摘要：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 SO2 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.
关键词：determination;HPLC;precolumn derivatization;shrimps;sulfites