摘要
目的:基于HPLC波长切换技术评价活血止痛胶囊中当归和乳香的质量。建立松香酸的检查方法,同时测定阿魏酸和11-羰基-β-乙酰乳香酸的含量。方法:色谱柱:Agilent TC-C_(18)(250 mm×4. 6 mm,5μm);柱温30℃;流动相:乙腈-0. 1%甲酸梯度洗脱(0～8 min:30%乙腈; 8～10 min:30%～80%乙腈; 10～30 min:80%乙腈; 30～40 min:30%乙腈);流速1. 0 mL·min^(-1);阿魏酸检测波长:321 nm;松香酸检测波长:240 nm; 11-羰基-β-乙酰乳香酸检测波长:250 nm。结果:松香酸检出限为3. 13 ng·mL^(-1)。阿魏酸和11-羰基-β-乙酰乳香酸分别在0. 01～100μg·mL^(-1)和0. 2～200μg·mL^(-1)范围内线性关系良好,平均回收率分别为99. 8%和102. 6%。3个厂家的9批样品阿魏酸含量在0. 20～0. 30 mg·g^(-1)之间,11-羰基-β-乙酰乳香酸含量在1. 96～3. 91 mg·g^(-1)之间。结论:所建方法准确、快速、简便,可为活血止痛胶囊的质量标准提高提供实验基础。
Objective: To evaluate the quality of Angelicae Sinensis Radix and Olibanum in Huoxue Zhitong capsules based on high performance liquid chromatography (HPLC) combined with wavelength switching. The testing method for abietic acid was established and the contents of ferulic acid and acetyl-11 -keto-p-boswellic acid were determined simultaneously. Methods: The separation was performed on an Agilent TC-C18 ( 250 inm × 4. 6 nun ,5 μm) column and the column temperature was set at 30℃. The mobile phase was composed of acetonitrile and 0. 1 % formic acid with gradient elution (0 ~ 8 min : 30% acetonitrile;8 ~ 10 min : 30%- 80% acetonitrile;10 .30 min : 80% acetonitrile) at a current speed of 1.0 mL·min^-1. The detection wavelengths were set at 321 nm for ferulic acid , 240 nm for abietic acid and 250 nm for acetyl-11-keto-β-boswellic acid , respectively. Results: The limit of detection of abietic acid was 3.13 ng. mL^-1. The calibration curves of ferulic acid and acetyl-11-keto- P-boswellic acid showed good linearity within the ranges of 0. 01 .100μg·mL^-1 and 0. 2 .200μg·mL^-1 , respectively. And the average recoveries for the above analytes were 99. 8% and 102. 6%, respectivelv. The contents of ferulic acid and acetyl-1keto-p-boswellic acid in 9 batches of samples from 3 manufactures were within 0. 20 - 0. 30 mg·g^-1 and 1.96 .3.91 mg·g^-1 ,respectively. Conclusion : The proposed method is accurate , rapid and simple, which provides scientific basis for improvement of the quality standard of Huoxue Zhitong capsules.
作者
聂黎行
戴忠
马双成
NIE Li-xing;DAI Zhong;MA Shuang-cheng(National Institutes for Food and Drug Control, Beijing 100050 , China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2019年第6期745-749,共5页
Chinese Journal of New Drugs
基金
国家自然科学基金资助项目(81303194)
中国食品药品检定研究院学科带头人培养基金资助项目(2017X1)
