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机构地区:[1]中南大学化学化工学院,长沙410083 [2]中南大学现代分析测试中心,长沙410083
出 处:《中国调味品》2012年第5期96-99,108,共5页China Condiment
摘 要:建立了一种柱前衍生高效液相色谱测定酱油中胱氨酸和半胱氨酸总含量的方法。以三丁基膦为还原剂,丙烯酸苄酯为衍生剂,醋酸铵、醋酸和甲醇的混合液为流动相,采用AQ-C18色谱柱分离,等度洗脱,流速为1.0mL/min,柱温为35℃,检测波长为257nm。通过对还原反应和衍生化反应中反应剂用量、反应温度、反应时间的研究,获得了优化的实验参数。结果显示在0.05~1.00mg/mL范围内具有良好的线性关系,r=0.9973(n=6),最低检出限为0.02mg/mL,平均回收率为98.70%~100.05%。此方法适用于酱油中(半)胱氨酸的检测,也为鉴别"毛发水酱油"提供了有效的检测手段。To establish a method of HPLC with pre-column derivation for determination of cystine and cysteine in soy sauce.The samples were reduced with tri-n-butylphosphine and derived with benzylacrylate.The mobile phase was ammonium acetate,acetic acid and methanol.The column was AQ-C18.The flow rate was 1.0 mL/min.Detection wavelength was 257 nm and the column temperature was 35 ℃.The experimental parameters that control reduction reaction and derivation reaction were studied and optimized,such as the response dose,reaction temperature,reaction time.The linear range was 0.05~1.00 mg/mL,r = 0.9973(n = 6),the limit of detection was 0.02 mg/mL.The average recovery was 98.70%~100.05%.The results showed that this method could be suitable for analysis of cystine and cysteine in soy sauce and could provide effective monitoring mersure for distinguish false soy sauce.
分 类 号:TS264.21[轻工技术与工程—发酵工程]
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