摘要
目的:建立HPLC波长切换法同时测定白益镇惊丸中的京尼平龙胆二糖苷、栀子苷、西红花苷-Ⅰ、去氢茯苓酸和茯苓酸5种活性成分的含量。方法:以十八烷基硅烷键合硅胶为填充剂,乙腈(A)-0.5%磷酸溶液(B)为流动相,进行梯度洗脱(0~11 min,15.0%A;11~22 min,15.0%A→28.0%A;22~31 min,28.0%A→45.0%A;31~42 min,45.0%A→70.0%A;42~50 min,70.0%A→15.0%A),流速0.9 m L·min-1,柱温30℃,波长切换法检测(0~22 min,238 nm,京尼平龙胆二糖苷和栀子苷;22~31 min,440 nm,西红花苷-Ⅰ;31~50 min,210 nm,去氢茯苓酸和茯苓酸),进样量为10μL。结果:京尼平龙胆二糖苷、栀子苷、西红花苷-Ⅰ、去氢茯苓酸和茯苓酸5种成分的质量浓度分别在5.930~118.6、11.41~228.2、4.950~99.00、4.100~82.00、4.780~95.60μg·m L-1呈现良好的线性关系,相关系数分别为0.9999、0.9998、0.9994、0.9999、0.9997;平均加样回收率及相应的RSD分别为99.42%(0.96%)、98.54%(1.08%)、99.06%(1.28%)、97.76%(0.84%)、98.19%(1.59%);供试品溶液在室温下12 h内稳定。结论:本文建立的HPLC波长切换法同时测定白益镇惊丸中的5种成分,该方法简便、稳定、可靠,可作为白益镇惊丸全面可靠的质量控制方法。
Objective： To develop an HPLC wavelength switching method for simultaneous determination of the contents of genipin-1-β-D-gentiobioside, geniposide, crocin-I, dehydropachymi cacid and pachymic acid in Baiyi Zhenjing Wan. Methods： Octadecyl silane bonded silica was used as filler, the mobile phase was acetonitrile（A）-0.5% phosphoric acid solution（B） with gradient elution（0-11 min, 15.0%A; 11-22 min, 15.0%A-28.0%A; 22-31 min, 28.0%A-45.0%A; 31-42 min, 45.0%A-70.0%A; 42-50 min, 70.0%A-15.0%A） at a flow rate of 0.9 m L·min-1, the column temperature was set at 30 ℃, and the detection wavelengths were 238 nm（genipin-1-β-D-gentiobioside and geniposide）, 440 nm（crocin-I）, 210 nm（dehydropachymic acid and pachymic acid）. Sample injection volume was 10 μL. Results： Genipin-1-β-D-gentiobioside, geniposide, crocin-I, dehydropachymic acid and pachymic acid had good linear relationships between the concentration and peak area in the ranges of 5.930-118.6 μg·m L-1（r=0.9999）, 11.41-228.2 μg·m L-1（r=0.9998）, 4.950-99.00（r=0.9994）, 4.100-82.00 μg·m L-1（r=0.9999）, and 4.780-95.60 μg·m L-1（r=0.9997）, respectively. The average recoveries and the corresponding RSDs were 99.42%（0.96%）, 98.54%（1.08%）, 99.06%（1.28%）, 97.76%（0.84%）, 98.19%（1.59%）, respectively. The sample solution was stable within 12 h at room temperature. Conclusion： An HPLC wavelength switching method has been successfully established for simultaneous determination of 5 components in Baiyi Zhenjing Wan. The established method is simple, accurate and reliable. The method is helpful for the quality control of Baiyi Zhenjing Wan.
出处
《中国药事》
CAS
2017年第3期275-280,共6页
Chinese Pharmaceutical Affairs
关键词
白益镇惊丸
京尼平龙胆二糖苷
栀子苷
西红花苷-Ⅰ
去氢茯苓酸
茯苓酸
波长切换法
多组分测定
Baiyi Zhenjing Wan
genipin-1-β-D-gentiobioside
geniposide
crocin-I
dehydropachymic acid
pachymic acid
wavelength switching method
multicomponent determination
