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HPLC-DAD法同时测定益肺清化颗粒的10种成分 被引量:1

Simultaneous determination of ten constituents in Yifei Qinghua Granules by HPLC-DAD
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摘要 目的建立HPLC-DAD法同时测定益肺清化颗粒中苦杏仁苷、齐墩果酸、熊果酸、仙鹤草酚B、甘草苷、毛蕊异黄酮葡萄糖苷、鲁斯可皂苷元、没食子酸、补骨脂素和紫菀酮的方法。方法采用反相液相色谱法,色谱柱为Waters Symmetry-C_(18)(250 mm×4.6 mm,5.0μm);流动相为KH2PO4缓冲溶液(KH2PO4 1.0 g,加水1 000 mL使溶解,磷酸调节p H值至3.5)-(乙腈-甲醇1∶1),梯度洗脱,体积流量0.8 mL/min;柱温40℃。结果苦杏仁苷、齐墩果酸、熊果酸、仙鹤草酚B、甘草苷、毛蕊异黄酮葡萄糖苷、鲁斯可皂苷元、没食子酸、补骨脂素和紫菀酮10种成分能够达到良好分离;其线性范围分别为0.2~2.0μg/mL(r=0.999 5)、0.4~4.0μg/mL(r=0.999 4)、0.3~3.0μg/mL(r=0.999 6)、0.1~1.0μg/mL(r=0.999 3)、0.5~5.0μg/mL(r=0.999 1)、0.15~1.50μg/mL(r=0.999 2)、0.25~2.50μg/mL(r=0.999 5)、0.6~6.0μg/mL(r=0.999 1)、0.45~4.50μg/mL(r=0.999 3)、0.12~1.20μg/mL(r=0.999 4),平均加样回收率分别为98.7%、98.0%、99.6%、98.0%、99.1%、99.4%、98.8%、101.1%、100.6%、101.7%,RSD分别为0.7%、1.3%、1.4%、1.4%、1.1%、0.8%、0.9%、0.5%、0.5%、0.8%。10批次供试品中苦杏仁苷、齐墩果酸、熊果酸、仙鹤草酚B、甘草苷、毛蕊异黄酮葡萄糖苷、鲁斯可皂苷元、没食子酸、补骨脂素和紫菀酮质量浓度分别为0.104~0.123、0.600~0.621、0.501~0.523、0.100~0.121、0.103~0.122、0.231~0.260、0.043~0.065、0.055~0.069、0.061~0.079、0.031~0.043 mg/g。结论本方法操作简便,结果准确可靠,可用于益肺清化颗粒的质量控制。 Objective To establish an HPLC-DAD method for the simultaneous determination of amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone in Yifei Qinghua Granules(YQG). Methods The chromatographic separation was achieved on an Waters Symmetry-C_(18)(250 mm × 4.6 mm, 5.0 μm) column with mobile phase consisted of(1.0 g potassium phosphate monobasic in 1 000 mL water, the p H value was adjusted to 3.5 with phosphate)-(acetonitrile-methanol 1∶1) for gradient elution, at the flow rate of 0.8 mL/min; The column temperature was 40 ℃. Results The linear ranges of amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone were 0.2—2.0 μg/mL(r = 0.999 4), 0.4—4.0 μg/mL(r = 0.999 4), 0.3—3.0 μg/mL(r = 0.999 6), 0.1—1.0 μg/mL(r = 0.999 3), 0.5—5.0 μg/mL(r = 0.999 1), 0.15—1.50 μg/mL(r = 0.999 2), 0.25—2.50 μg/mL(r = 0.999 5), 0.6—6.0 μg/mL(r = 0.999 1), 0.45—4.50 μg/mL(r = 0.999 3), and 0.12—1.20 μg/mL(r = 0.999 4), respectively. These ten components were well resolved. Their average recoveries(n = 6) respectively were 98.7%(RSD = 0.7%), 98.0%(RSD = 1.3%), 99.6%(RSD = 1.4%), 98.0%(RSD = 1.4%), 99.1%(RSD = 1.1%), 99.4%(RSD = 0.8%), 98.8%(RSD = 0.9%), 101.1%(RSD = 0.5%), 100.6%(RSD = 0.5%), and 101.7%(RSD = 0.8%). The content of ten batches of the amygdalin, oleanolic acid, ursolic acid, agrimol B, liquiritin, calycosin-7-glucoside, ruscogenin, gallic acid, psoralen, and shionone was 0.104—0.123, 0.600—0.621, 0.501—0.523, 0.100—0.121, 0.103—0.122, 0.231—0.260, 0.043—0.065, 0.055—0.069, 0.061—0.079, 0.031—0.043 mg/g, respectively. Conclusion The method is accurate, sensitive, credible, and repeatable, which can be applied to the quality control of YQG.
作者 钱钧强 朱宏明 房志仲 潘占宇 QIAN Jun-qiang1, ZHU Hong-ming2, FANG Zhi-zhong3, PAN Zhan-yu1,( 1. Tianjin Key Laboratory of Cancer Prevention and Therapy, Tianjin Clinical Research Center for Cancer, National Clinical Research Center for Cancer, Department of Pharmacy, Tianjin Medical University Cancer Institute and Hospital, Tianjin 300060, China; 2. Tianjin Medical University Zhongxin Eco-city Hospital, Tianjin 300467, China ;3. College of Pharmacy, Tianjin Medical University, Tianjin 300070, China)
出处 《中草药》 CSCD 北大核心 2018年第19期4561-4566,共6页 Chinese Traditional and Herbal Drugs
关键词 益肺清化颗粒 HPLC-DAD 质量控制 苦杏仁苷 齐墩果酸 熊果酸 仙鹤草酚B 甘草苷 毛蕊异黄酮葡萄糖苷 鲁斯可皂苷元 没食子酸 补骨脂素 紫菀酮 Yifei Qinghua Granules HPLC-DAD quality control amygdalin oleanolic acid ursolic acid agrimol B liquiritin calycosin-7-glucoside ruscogenin gallic acid psoralen shionone
作者简介 钱钧强,男,研究方向为医院药学。Tel:(022)23340123 E-mail:lvn1314@126.com;通信作者潘占宇,男,主任医师,研究方向为中西医结合临床治疗。Tel:(022)23340123
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