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投稿时间:2024-04-04
投稿时间:2024-04-04
中文摘要: 该研究建立一种高效且准确测定酱油生物胺含量的超高效液相色谱(ultra performance liquid chromatography,UPLC)方法。酱油成分复杂,影响生物胺含量检测的因素较多。为得到较为准确的生物胺含量,选择不同的酸性提取剂、提取方式和时间以及衍生温度、衍生时间和衍生剂体积作为酱油前处理优化试验的条件,经多次试验建立测定酱油中色胺、苯乙胺、腐胺、尸胺、组胺、酪胺、亚精胺、精胺8 种生物胺含量的UPLC 方法。结果表明,采用5%三氯乙酸作为提取剂、样品超声辅助提取30 min、加入1 mL 衍生剂42 ℃衍生45 min 为最佳条件。8 种生物胺可在26 min 内分离,且在2.5~50.0 mg/L 线性良好,相关性系数R2 为0.996 4~0.999 5,检出限为0.02~0.15 mg/L,定量限为0.10~0.75 mg/L,样品平均加标回收率为72.00%~122.53%,相对标准偏差(relative standard deviation,RSD)为0.78%~12.23%。方法学试验表明该研究建立的方法灵敏度较高,结果较准确,可以满足酱油中生物胺的定性定量分析要求。
Abstract:This study established an efficient and accurate ultra performance liquid chromatography (UPLC)method for the determination of biogenic amines in soy sauce. The composition of soy sauce is complex,and there are many factors affecting the detection of biogenic amine content. In order to obtain a more accurate biogenic amine content,different acidic extractants,extraction methods and time,as well as derivative temperature,derivative time and derivative agent volume were selected as the conditions for the optimization test of soy sauce pretreatment. A UPLC method for the determination of tryptamine,phenylethylamine,putrescine,cadaverine,histamine,tyramine,spermidine and spermine in soy sauce was established by multiple experiments.The results showed that the optimum conditions were as follows 5% trichloroacetic acid as extractant,ultrasonicassisted extraction for 30 min,and derivatization at 42 ℃ for 45 min with 1 mL derivatization agent. The eight biogenic amines could be separated within 26 min,and the linearity was good in the range of 2.5-50.0 mg/L.The correlation coefficient R2 was 0.996 4-0.999 5,the detection limit was 0.02-0.15 mg/L,and the limit of quantitation was 0.10-0.75 mg/L. The average spiked recovery of the samples was 72.00%-122.53%,and the relative standard deviation (RSD) was 0.78%-12.23%. The methodological test showed that the method established in this study had high sensitivity and accurate results,which could meet the requirements of qualitative and quantitative analysis of biogenic amines in soy sauce.
keywords: soy sauce biogenic amines extraction ultra-performance liquid chromatography (UPLC) detection methods
文章编号:202514019 中图分类号: 文献标志码:
基金项目:国家自然科学基金项目(32072198、32302023、32372284);广东省自然科学基金项目(2023A1515012536、2021B1515120042、2022A1515140021);广东省教育厅项目(2021KCXTD034、2023KTSCX131)
| Author Name | Affiliation |
| CAI Yuming,LIU Muzhuang,HUANG Guidong,WANG Ali,ZHONG Xianfeng,HONG Jiazhi,WEN Haixiang * | Foshan University,Foshan 528000,Guangdong,China |
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