论文部分内容阅读
建立肉制品中栀子黄色素中藏花素和藏花酸残留的高效液相色谱串联质谱(HPLC-MS/MS)分析方法。实验优化了样品提取方法、液相色谱条件和质谱参数。样品用甲醇超声提取,乙腈饱和的正己烷脱脂,Eclipose plus C18色谱柱分离,流动相为乙腈-水溶液,流速1.0 m L/min。采用电喷雾质谱负离子模式电离,多重反应选择离子检测。藏花素的检测离子对为m/z 975.4/651.3和m/z 975.4/327.1,其中定量离子对为m/z 975.4/651.3,藏花酸的检测离子对为m/z 327.2/105.0和m/z 327.2/185.1,其中定量离子对为m/z 327.2/105.0。结果表明,线性范围50~2000 ng/m L,回收率为80.49%~90.34%,相对标准偏差<3.01%,藏花素和藏花酸的仪器检出限分别为5、3 ng/m L,方法定量限分别为20、12 ng/m L,该方法简单、准确,适用于肉制品中栀子黄色素的定量检测。
To establish a HPLC-MS / MS method for the determination of crocin and crocin in gardenia yellow in meat products. Experiments optimized sample extraction methods, LC conditions and MS parameters. Samples were extracted with methanol, acetonitrile-saturated n-hexane, and separated on an Eclipose plus C18 column. The mobile phase was acetonitrile-water at a flow rate of 1.0 mL / min. Electrospray mass spectrometry negative ion mode ionization, multiple reaction selective ion detection. The detection ion pair of crocin was m / z 975.4 / 651.3 and m / z 975.4 / 327.1, of which the quantitative ion pair was m / z 975.4 / 651.3 and the crocetin ion was m / z 327.2 / 105.0 and m / z 327.2 / 185.1, where the quantitative ion pair is m / z 327.2 / 105.0. The results showed that the linear range was 50-2000 ng / m L, the recoveries were 80.49% -90.34%, and the relative standard deviations were less than 3.01%. The detection limits of crocin and hsAC were 5,3 ng / m L , The limit of quantification was 20 and 12 ng / mL, respectively. The method was simple and accurate and was suitable for the quantitative determination of gardenia yellow in meat products.