酱油中胱氨酸的高效液相色谱-串联质谱法测定Determination of Cystine in Soy Sauce by High Performance Liquid Chromatography-Mass Spectrometry
蒋林蓉,徐志伟,程立媛,徐彬,卓海华,王玉健
摘要(Abstract):
采用高效液相色谱-串联质谱技术建立了酱油中胱氨酸的分析方法。酱油样品用甲醇-水为提取溶液,加入乙二胺-N-丙级硅烷(PSA)和十八烷基硅烷(C18)吸附剂除去杂质,无需衍生化处理,采用亲水作用色谱(HILIC)柱,以乙腈/0.1%甲酸水溶液为流动相梯度洗脱进行液相色谱分离。结果显示在0.02~0.12μg/mL具有良好的线性关系,r=0.9996。方法的检出限(LODs,信噪比为3)在0.15mg/kg,定量下限(LOQs,信噪比为10)为0.5mg/kg。在生抽和老抽两种阴性基质中3个加标水平的回收率都在82.8%~108.2%,加标含量范围在0.5~1.0mg/kg,相对标准偏差(RSD,n=8)在1.19%~7.57%。方法的前处理简便,灵敏度和回收率高,选择性好,适用于酱油中胱氨酸含量的检测,也为鉴别"毛发水酱油"提供了有效检测手段。
关键词(KeyWords): 液相色谱-串联质谱;胱氨酸;酱油;测定
基金项目(Foundation): 海南省自然科学基金项目(313105);海南省自然科学基金项目(203128)
作者(Author): 蒋林蓉,徐志伟,程立媛,徐彬,卓海华,王玉健
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