引用本文: | 高森,白雪,文柳静,王鑫,李正翔,房志仲.HPLC波长切换联合梯度洗脱法同时测定参苏宣肺丸中的6种成分[J].中国现代应用药学,2016,33(10):1300-1304. |
| GAO Sen,BAI Xue,WEN Liujing,WANG Xin,LI Zhengxiang,FANG Zhizhong.Determination of Six Components in Shensu Xuanfei Wan by HPLC with Wavelength Switching Combined Gradient Elution Method[J].Chin J Mod Appl Pharm(中国现代应用药学),2016,33(10):1300-1304. |
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HPLC波长切换联合梯度洗脱法同时测定参苏宣肺丸中的6种成分 |
高森1, 白雪2, 文柳静3, 王鑫1, 李正翔1, 房志仲4
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1.天津医科大学总医院药剂科, 天津 300052;2.天士力控股集团研究院中药开发中心, 创新中药关键技术国家重点实验室, 天津 300402;3.天津医科大学肿瘤医院药学部, 国家肿瘤临床医学研究中心, 天津市"肿瘤防治"重点实验室, 天津 300060;4.天津医科大学药学院, 天津市临床药物关键技术重点实验室, 天津 300070
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摘要: |
目的 建立HPLC波长切换联合梯度洗脱法同时测定参苏宣肺丸中咖啡酸、迷迭香酸、3’-羟基葛根素、葛根素、3’-甲氧基葛根素、大豆苷的含量。方法 采用ZOBAX SB-C18色谱柱(4.6 mm×250 mm,5 μm);流动相A为甲醇-乙腈(1:1),流动相B为0.1%冰醋酸溶液,进行梯度洗脱;流速为1.0 mL·min-1;咖啡酸和迷迭香酸的检测波长为320 nm,3’-羟基葛根素、葛根素、3’-甲氧基葛根素和大豆苷的检测波长为250 nm;进样量为20 μL。结果 咖啡酸、迷迭香酸、3’-羟基葛根素、葛根素、3’-甲氧基葛根素、大豆苷的浓度与峰面积分别在2.32~46.40 μg·mL-1(r=0.999 8)、3.06~61.20 μg·mL-1(r=0.999 5)、4.45~89.00 μg·mL-1(r=0.999 9)、14.48~289.60 μg·mL-1(r=0.999 9)、4.86~97.20 μg·mL-1(r=0.999 7)、3.69~73.80 μg·mL-1(r=0.999 6)内具有较好的线性关系,平均加样回收率和相应的RSD分别为99.0%(1.6%),97.5%(0.6%),99.3%(0.9%),98.6%(1.3%),97.6%(1.3%),97.0%(0.9%)。结论 方法操作准确、简便,可用于参苏宣肺丸的质量控制。 |
关键词: HPLC 波长切换联合梯度洗脱法 参苏宣肺丸 咖啡酸 迷迭香酸 3'-羟基葛根素 葛根素 3'-甲氧基葛根素 大豆苷 |
DOI:10.13748/j.cnki.issn1007-7693.2016.10.019 |
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Determination of Six Components in Shensu Xuanfei Wan by HPLC with Wavelength Switching Combined Gradient Elution Method |
GAO Sen1, BAI Xue2, WEN Liujing3, WANG Xin1, LI Zhengxiang1, FANG Zhizhong4
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1.Department of Pharmacy, General Hospital, Tianjin Medical University, Tianjin 300052, China;2.Tasly Holding Group Academy of Traditional Chinese Medicine Development Center, State Key Laboratory of Chinese Medicine Key Technology Innovation, Tianjin 300402, China;3.Department of Pharmacy, Tianjin Medical University Cancer Hospital, State Cancer Clinical Medical Research Center, Tianjin Key Lab of Cancer Prevention and Treatment, Tianjin 300060, China;4.College of Pharmacy, Tianjin Medical University, Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics(Theranostics), Tianjin 300070, China
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Abstract: |
OBJECTIVE To develop an HPLC with wavelength switching combined gradient elution method for simultaneous determination of caffeic acid, rosmarinic acid, 3'-hydroxy puerarin, puerarin, 3'-methoxypuerarin and daidzin in Shensu Xuanfei Wan. METHODS ZOBAX SB-C18 column (4.6 mm×250 mm,5 μm) was applied with methanol-acetonitrile (1:1) (A) and 0.1% glacial acetic acid solution(B) as mobile phase in gradient mode. The flow rate was 1.0 mL·min-1. Caffeic acid and rosmarinic acid were detected at 320 nm, 3'-hydroxy puerarin, puerarin, 3'-methoxypuerarin and daidzin were detected at 250 nm. Injection volume was 20 μL. RESULTS The concentration and peak area of caffeic acid, rosmarinic acid, 3'-hydroxy puerarin, puerarin, 3'-methoxypuerarin and daidzin were at 2.32~46.40 μg·mL-1(r=0.999 8), 3.06~61.20 μg·mL-1 (r=0.999 5), 4.45~89.00 μg·mL-1(r=0.999 9), 14.48~289.60 μg·mL-1(r=0.999 9), 4.86~97.20 μg·mL-1(r=0.999 7), 3.69~73.80 μg·mL-1 (r=0.999 6), respectively, and showed a good linear relationship. The average recoveries and the corresponding RSD were 99.0%(1.6%), 97.5% (0.6%), 99.3%(0.9%), 98.6%(1.3%), 97.6%(1.3%), 97.0%(0.9%), respectively. CONCLUSION The method is accurate, quick, simple. It could be reliable for the quality control of Shensu Xuanfei Wan. |
Key words: HPLC wavelength switching combined gradient elution method Shensu Xuanfei Wan caffeic acid rosmarinic acid 3'-hydroxy puerarin puerarin 3'-methoxypuerarin daidzin |
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