摘要
试验建立了通过质量吸收系数校准羟基-α-山椒素工作液浓度的方法,解决了花椒麻素标准品不稳定的问题;建立了以羟基-α-山椒素为标样同时测定花椒及其提取物中羟基-ε-山椒素、羟基-α-山椒素、羟基-β-山椒素和羟基-γ-山椒素的高效液相色谱方法,方法采用Agilent Zorbax SB-C18 (4.6 mm×100 mm, 5μm)色谱柱,流动相为乙腈-1%冰醋酸水(40︰60, V/V),流速为1.5 mL/min,检测波长为270 nm,柱温为40℃。羟基-α-山椒素在0.007 84~0.078 4 mg/mL范围内与峰面积呈良好的线性关系, R2为0.999 8,花椒和花椒提取物的花椒麻素检出限分别为0.005 mg/g和0.05 mg/g,在14.4~54 mg/g范围内加标平均回收率为99.75%,样品检测RSD (N=9)均在1.5%以内。试验评价了三种不同产地和品种的花椒样品,通过对花椒麻素的组成进行分析,得出不同产地和品种的花椒中各种花椒麻素成分比例具有特征性,羟基-γ-山椒素成分比例可以作为鉴别不同产地和品种的特征指标。
A method was established to calibrate the concentration of hydroxyl-α-sanshool working solution by mass absorption coefficient,and it could solve the problem of unstable of Chinese sanshool standard.A high performance liquid chromatography was established tomeasurehydroxyl-ε-sanshool,hydroxyl-α-sanshool,hydroxyl-β-sanshool and hydroxyl-γ-sanshool by using hydroxyl-α-sanshoolstandard.Agilent Zorbax SB-C18 column(150 mm×4.6 mm,5μm)was used as chromatographic column,eluted by the mobile phase of acetonitrile-1%glacial acetic water(V/V=40︰60)with a flow rate of 1.5 mL/min,and a detection wavelength of 270 nm,and column temperature was 40℃.The linear range of hydroxyl-α-sanshool was0.007 84-0.078 4 mg/mL with R2 value of 0.999 8,the average recovery rate was 99.75%in the range from14.4 to 54 mg/g,and the sample test RSD(N=9)was within 1.5%.Three different habitats and varieties of Sichuan pepper samples were evaluated.Through the analysis of ingredient compositions of sanshool,it was concluded that different habitats and varieties of Sichuan pepper had different characteristics in sanshool composition,and hydroxyl-γ-sanshool could be used as identification characteristics of different habitats and varieties.
作者
杨清山
翟彦伟
栗星
李松松
钱建瑞
YANG Qingshan;ZHAI Yanwei;LI Xing;LI Songsong;QIAN Jianrui(Engineering Research Center of Natural Pigment in Hebei Province,Handan 057250;Chenguang Biotech Group Co.,Ltd.,Handan 057250;Hebei Chenguang Testing Service Co.,Ltd.,Handan 057250)
出处
《食品工业》
CAS
北大核心
2019年第8期328-332,共5页
The Food Industry
基金
河北省科技条件建设项目（中央引导地方科技创新专项资金）（169676405G），香辛料精油连续精馏提取关键技术及装备研发
