| 郑晓萍,杨晓娟,杨自荣,李小玲,吕仁,班小军,黄秀霞.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[J].中国药事,2017,(3):275-280 |
| 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 |
| Simultaneous Determination of Genipin-1-β-D-gentiobioside, Geniposide, Crocin-I, Dehydropachymic Acid and Pachymic Acid in Baiyi Zhenjing Wan by HPLC Wavelength Switching Method |
| 投稿时间：2016-08-17 |
| DOI：10.16153/j.1002-7777.2017.03.008 |
| 中文关键词: 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 |
| 英文关键词: Baiyi Zhenjing Wan genipin-1-β-D-gentiobioside geniposide crocin-I dehydropachymic acid pachymic acid wavelength switching method multicomponent determination |
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| 中文摘要: |
| 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 mL·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10 μL。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、4.780~95.60 μg·mL-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。 |
| 英文摘要: |
| 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 mL·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·mL-1(r=0.9999), 11.41-228.2 μg·mL-1(r=0.9998), 4.950-99.00 (r=0.9994), 4.100-82.00 μg·mL-1(r=0.9999), and 4.780-95.60 μg·mL-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. |
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