By optimizing the separation and analytical conditions, a reliable, simple and accurate high-performance liquid chromatography（HPLC） method coupled with ultraviolet（UV） and evaporative light scattering detector（E...By optimizing the separation and analytical conditions, a reliable, simple and accurate high-performance liquid chromatography（HPLC） method coupled with ultraviolet（UV） and evaporative light scattering detector（ELSD） was developed for the simultaneous determination of lactones and flavonoid, that is, bilobalide, ginkgolide A, ginkgolide B, and rutin, in more than 10 batches of Ginkgo biloba tablets from different pharmaceutical companies. The method could also be applied to fingerprint research, for a more general evaluation of the quality of this preparation. The separation of the components was achieved on a Hanbon C18 column with gradient elution using water and methanol containing 0.1% trifluoroacetic acid（TFA）. The column temperature was 30 ℃ and the flow-rate of the mobile phase was 0.6 mL/min. The drift tube temperature of the ELSD was set at 100 ℃, and the nitrogen flow-rate was 2 L/min. Good linear relationships were shown with correlation coefficients for analytes exceeding 0.9913. The limits of detection（LODs, S/N=3） and the limits of quantitation（LOQs, S/N=10） were 0.00887-0.0508 μg/μL and 0.0171- 0.0636 μg/μL, respectively, on the column. The relative standard deviations（RSD） of the analytes were less than 3.61% for intraday and 3.70% for interday, respectively. The average recovery rates obtained were in the range of （97.3±4.3）% to （101.9±3.1）% for all the compounds. The results of quantitative and fingerprint analysis proved that the contents of the components were totally similar in the preparation of Ginkgo biloba tablets from the same pharmaceutical company; whereas, they varied significantly in the preparations of Ginkgo biloba tablets from different companies.展开更多
目的建立泽泻的HPLC-UV指纹图谱,为科学评价泽泻的质量提供依据。方法使用Agilent ZORBAX Eclipse Plus C18色谱柱(250mm×4.6mm,5μm);柱温为30℃;流速为1mL·min-1;检测波长为210nm;乙腈-水为流动相进行梯度洗脱。对11批泽泻...目的建立泽泻的HPLC-UV指纹图谱,为科学评价泽泻的质量提供依据。方法使用Agilent ZORBAX Eclipse Plus C18色谱柱(250mm×4.6mm,5μm);柱温为30℃;流速为1mL·min-1;检测波长为210nm;乙腈-水为流动相进行梯度洗脱。对11批泽泻进行指纹图谱相似度研究。结果建立了泽泻的HPLC-UV指纹图谱方法,精密度、重复性和稳定性均良好,指纹图谱指认了环氧泽泻烯和23-乙酰泽泻醇B色谱峰,11批泽泻的指纹图谱相似度均大于0.85。结论该方法简便、可靠、重复性好,可为泽泻的质量控制及评价提供科学依据。展开更多
基金Supported by the Program for New Century Excellent Talents in University of China(No.NCET-06-0515).
文摘By optimizing the separation and analytical conditions, a reliable, simple and accurate high-performance liquid chromatography（HPLC） method coupled with ultraviolet（UV） and evaporative light scattering detector（ELSD） was developed for the simultaneous determination of lactones and flavonoid, that is, bilobalide, ginkgolide A, ginkgolide B, and rutin, in more than 10 batches of Ginkgo biloba tablets from different pharmaceutical companies. The method could also be applied to fingerprint research, for a more general evaluation of the quality of this preparation. The separation of the components was achieved on a Hanbon C18 column with gradient elution using water and methanol containing 0.1% trifluoroacetic acid（TFA）. The column temperature was 30 ℃ and the flow-rate of the mobile phase was 0.6 mL/min. The drift tube temperature of the ELSD was set at 100 ℃, and the nitrogen flow-rate was 2 L/min. Good linear relationships were shown with correlation coefficients for analytes exceeding 0.9913. The limits of detection（LODs, S/N=3） and the limits of quantitation（LOQs, S/N=10） were 0.00887-0.0508 μg/μL and 0.0171- 0.0636 μg/μL, respectively, on the column. The relative standard deviations（RSD） of the analytes were less than 3.61% for intraday and 3.70% for interday, respectively. The average recovery rates obtained were in the range of （97.3±4.3）% to （101.9±3.1）% for all the compounds. The results of quantitative and fingerprint analysis proved that the contents of the components were totally similar in the preparation of Ginkgo biloba tablets from the same pharmaceutical company; whereas, they varied significantly in the preparations of Ginkgo biloba tablets from different companies.
文摘目的建立泽泻的HPLC-UV指纹图谱,为科学评价泽泻的质量提供依据。方法使用Agilent ZORBAX Eclipse Plus C18色谱柱(250mm×4.6mm,5μm);柱温为30℃;流速为1mL·min-1;检测波长为210nm;乙腈-水为流动相进行梯度洗脱。对11批泽泻进行指纹图谱相似度研究。结果建立了泽泻的HPLC-UV指纹图谱方法,精密度、重复性和稳定性均良好,指纹图谱指认了环氧泽泻烯和23-乙酰泽泻醇B色谱峰,11批泽泻的指纹图谱相似度均大于0.85。结论该方法简便、可靠、重复性好,可为泽泻的质量控制及评价提供科学依据。
