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作 者:易小丽[1] 周昭娟 王丽达 张杰[1] 芦楠[1] 白若石[1] YI Xiaoli;ZHOU Zhaojuan;WANG Lida;ZHANG Jie;LU Nan;BAI Ruoshi(Beijing Research Station of Technical Center,Shanghai Tobacco Group Co.,Ltd.,Beijing 100121,China)
机构地区:[1]上海烟草集团有限责任公司技术中心北京工作站,北京100121
出 处:《理化检验(化学分册)》2019年第1期78-82,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:取经烘干并粉碎的烟叶样品0.100 0g,加入CH_3OH-H_2O(1+1)混合液20mL,超声提取20min。提取液经0.45μm滤膜过滤,滤液供高效液相色谱法分析。以Diamonsil Plus C_(18)色谱柱为固定相,并用不同比例的(A)甲醇和(B)乙酸-水(1+99)溶液的混合液按设定程序进行梯度洗脱,使样品中的绿原酸及其异构体分离。采用紫外检测器进行检测。结果表明:绿原酸的线性范围在1.01~101.22mg·L^(-1)之间,其异构体(新绿原酸及隐绿原酸)则同在0.25~25.00mg·L^(-1)之间,其检出限(3S/N)分别为0.013,0.025,0.028mg·L^(-1)。按标准加入法进行回收试验,测得回收率在92.0%~104%之间,测定值的相对标准偏差(n=5)在1.1%~4.0%之间。A portion of dried and powdered tobacco leaf sample(0.100 0 g)was extracted ultrasonically with 20 mL of CH3OH-H2O(1+1)mixture for 20 min.The extract obtained was filtered through 0.45μm filtering membrane and the filtrate was used for HPLC analysis.Diamonsil Plus C18 column was used as stationary phase and mixtures of(A)methanol and(B)CH3COOH(1+99)solution in various proportions were used as mobile phase in the programmed gradient elution,to have chlorogenic acid and its isomers(neochlorogenic acid and cryptochlorogenic acid)clearly separated.It was shown that linearity range for chlorogenic acid was found between 1.01-101.22 mg·L^-1,while those for its isomers(i.e.,neochlorogenic acid and cryptochlorogenic acid)were found same between 0.25-25.00 mg·L^-1,and that values of detection limits(3 S/N)for the 3 compounds were 0.013,0.025,0.028 mg·L^-1 respectively.Test for recovery was made by standard addition method,giving values of recovery in the range from 92.0%to 104%,and RSDs(n=5)in the range from 1.1%to 4.0%.
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