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机构地区:[1]青海省食品药品检验所,西宁810016 [2]扬子江药业集团北京海燕药业有限公司,北京102206
出 处:《中华中医药杂志》2013年第2期544-547,共4页China Journal of Traditional Chinese Medicine and Pharmacy
基 金:青海省科技计划项目(No.2012-Z-736)~~
摘 要:目的:建立测定大籽獐牙菜中1-羟基-3,7,8-三甲氧基酮、1,5,8-三羟基-3-甲氧基酮、1,8-二羟基-3,7-二甲氧基酮、1,7-二羟基-3,8-二甲氧基酮4种酮类成分含量的HPLC方法。方法:采用Zorbax SB-C18色谱柱(4.6mm×250mm,5μm),以甲醇-水进行梯度洗脱(0min,65:35;50min,70:30;50.1min,65:35;60min,65:35);流速:1.0mL/min;检测波长:254nm;柱温:30℃。结果:1-羟基-3,7,8-三甲氧基酮、1,5,8-三羟基-3-甲氧基酮、1,8-二羟基-3,7-二甲氧基酮、1,7-二羟基-3,8-二甲氧基酮的线性范围分别为(0.0173-0.8640)μg,(0.0623-3.1200)μg,(0.0305-3.0500)μg和(0.0562-5.6200)μg,相关系数r分别为0.9997,0.9999,0.9998和0.9999,其平均回收率(n=5)分别为100.1%,99.7%,100.5%,99.7%,RSD分别为1.1%,1.3%,1.2%,1.5%。结论:本方法可用于大籽獐牙菜的质量控制。Objective: To develop a high performance liquid chromatography method for simultaneous determination of four major xanthones present in Swertia macrosperma C.B.Clark. Methods: The analysis was achieved on an Zorbax SB-C18 column(4.6mm×250mm, 5μm) using a mobile phase of methanol-water gradient elution in a total run time of 60min(0min, 65:35; 50min, 70:30; 50.1min, 65:35; 60rain, 65:35), with detected wavelength 254nrn, flow rate at 1.0mL/min, column temperature 30% Results: 1-hydroxy-3,7,8-trimethoxyxanthone, 1,5,8-trihydroxy-3-methoxy-xanthone, 1,8-dihydroxy-3,7-dimethoxyxanthone, 1,7-dihydroxy-3,8-dimethoxyxanthone were linear over the range of 0.0173-0.8640μg, 0.0623-3.12001xg, 0.0305-3.0500μg, 0.0562-5.6200μg with coefficients (r) of 0.9997, 0.9999, 0.9998, 0.9999 respectively. The average recoveries (n=5) were 100.1%, 99.7%, 100.5%, 99.7%, with RSD of 1.1%, 1.3%, 1.2%, 1.5%, respectively. Conclusion: This method is simple, sensitive, reliable and reproducible. It can be applied to study the quality control of Swertia macrosperma C.B.Clark.
关 键 词:大籽獐牙菜 1-羟基-3 7 8-三甲氧基酮 1 5 8-三羟基-3-甲氧基酮 1 8-二羟基-3 7-二甲氧基酮 1 7-二羟基-3 8-二甲氧基酮 高效液相色谱法
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