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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
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
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-1r=0.999 8)、3.06~61.20 μg·mL-1r=0.999 5)、4.45~89.00 μg·mL-1r=0.999 9)、14.48~289.60 μg·mL-1r=0.999 9)、4.86~97.20 μg·mL-1r=0.999 7)、3.69~73.80 μg·mL-1r=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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基金项目:
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
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
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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