牡丹花粉口含片的质量标准研究
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摘要
目的:建立牡丹花粉口含片的质量控制方法,为其质量标准的拟定提供参考。方法:按2015年版《中国药典》(四部)薄层色谱(TLC)法对牡丹花粉口含片中的芍药苷、山柰酚、木犀草素进行定性鉴别;采用双波长-高效液相色谱(HPLC)法对牡丹花粉口含片中的芍药苷和氧化芍药苷进行定量分析[色谱柱为Agilent TC-C_(18);流动相为乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱;流速为1.0 mL/min;检测波长芍药苷为230 nm、氧化芍药苷为258 nm;进样量为20μL]。结果:芍药苷、山柰酚、木犀草素的TLC鉴别结果显示,在样品图谱中,与对照品图谱相应位置上均显相同颜色的特征斑点,且阴性对照无干扰。芍药苷和氧化芍药苷的检测质量浓度分别在7.2～86.4、2.72～32.64μg/mL范围内与各自峰面积呈良好的线性关系(r≥0.999 7);平均加样回收率分别为99.12%、98.65%,RSD分别为1.54%、2.53%(n=6);精密度(n=6)、稳定性(n=8)、重复性(n=6)试验的RSD均小于3.0%。结论:该方法操作简便、重复性好,可用于牡丹花粉口含片的质量控制。
OBJECTIVE:To establish a method for quality control of Peony pollen buccal tablets,and to provide reference for the formulation of quality standard. METHODS:TLC method was used for qualitative identification of paeoniflorin,kaempferol and luteolin in Peony pollen buccal tablets according to 2015 edition of Chinese Pharmacopeia(part Ⅳ). The contents of paeoniflorin and oxypaeoniflorin in Peony pollen buccal tablets were determined by dual-wavelength HPLC method [The determination was perform on Agilent TC-C_(18) column with mobile phase consisted of acetonitrile(A)-0.1% phosphoric acid solution(B)with gradient elution at the flow rate of 1.0 m L/min. The detection wavelength was set at 230 nm for paeoniflorin and 258 nm for oxypaeoniflorin. Sample size was 20 μL]. RESULTS:TLC identification of paeoniflorin,kaempferol and luteolin showed that the same color characteristic spots of control chromatogram appeared in the corresponding positions of sample chromatogram without interference from negative samples. The linear range of paeoniflorin and oxypaeoniflorin were 7.2-86.4μg/mL and 2.72-32.64 μg/mL(r≥0.999 7),respectively. The average recoveries were 99.12% and 98.65%,and RSD were 1.54% and 2.53%(n=6),respectively. RSDs of precision(n=6),stability(n=8)and reproducibility(n=6)tests were all lower than 3.0%. CONCLUSIONS:The method is simple and reproducible,and can be used for quality control of Peony pollen buccal tablets.
OBJECTIVE:To establish a method for quality control of Peony pollen buccal tablets,and to provide reference for the formulation of quality standard. METHODS:TLC method was used for qualitative identification of paeoniflorin,kaempferol and luteolin in Peony pollen buccal tablets according to 2015 edition of Chinese Pharmacopeia(part Ⅳ). The contents of paeoniflorin and oxypaeoniflorin in Peony pollen buccal tablets were determined by dual-wavelength HPLC method [The determination was perform on Agilent TC-C_(18) column with mobile phase consisted of acetonitrile(A)-0.1% phosphoric acid solution(B)with gradient elution at the flow rate of 1.0 m L/min. The detection wavelength was set at 230 nm for paeoniflorin and 258 nm for oxypaeoniflorin. Sample size was 20 μL]. RESULTS:TLC identification of paeoniflorin,kaempferol and luteolin showed that the same color characteristic spots of control chromatogram appeared in the corresponding positions of sample chromatogram without interference from negative samples. The linear range of paeoniflorin and oxypaeoniflorin were 7.2-86.4μg/mL and 2.72-32.64 μg/mL(r≥0.999 7),respectively. The average recoveries were 99.12% and 98.65%,and RSD were 1.54% and 2.53%(n=6),respectively. RSDs of precision(n=6),stability(n=8)and reproducibility(n=6)tests were all lower than 3.0%. CONCLUSIONS:The method is simple and reproducible,and can be used for quality control of Peony pollen buccal tablets.
引文
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[14]李盈,王举涛,刘金旗,等.HPLC法同时测定牡丹皮中芍药苷和氧化芍药苷含量[J].亚太传统医药,2016,12(21):25-27.
[15]欧金梅,吴德玲,金传山,等.HPLC法同时测定白芍总苷中4种单萜苷的含量[J].中药材,2013,36(3):423-425.
[16]何秀菊,张振秋,王婧宁,等.HPLC波长切换法同时测定桂枝、白芍药对提取物中8个成分的含量[J].药物分析杂志,2013,33(11):1899-1903.
[17]周军,张蕾,王杰.HPLC-DAD法测定脑血栓片中苦杏仁苷、羟基红花黄色素A、芍药苷、阿魏酸、丹酚酸B和丹参酮ⅡA[J].现代药物与临床,2015,30(3):262-266.
[18]严玉平,由会玲,李国川,等.芍药及不同炮制品在芍药甘草汤中芍药苷含量的差异研究[J].中国药房,2009,20(6):463-465.
[2]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:158,172.
[3]王斌利,王新娣,董颖,等.牡丹的食药价值研究进展[J].甘肃医药,2017,36(2):96-97.
[4]张孟琴,孙亚真,范一霖.牡丹花粉营养成分评价及相关性分析[J].食品研究与开发,2018,39(15):154-160.
[5]何得平.临夏油用紫斑牡丹花粉营养成分分析[J].林业实用技术,2017(3):57-58.
[6]邵帅.油菜及牡丹花粉抗良性前列腺增生活性成分分析[D].南京:南京农业大学,2015.
[7]林昌永.白芍总苷治疗NIH-Ⅲ型前列腺炎效果观察[J].中国乡村医药,2017,24(4):45-46.
[8]王浩,周玉春,薛建国.中药有效成分治疗慢性前列腺炎的免疫机制[J].中华男科学杂志,2016,22(1):63-66.
[9]石晓峰,范彬,李运,等.一种牡丹花粉口含片及其制备方法:中国,201710254599.5[P].2017-08-18.
[10]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:57.
[11]王英,王路华,付丽萍,等.抗宫炎片质量标准研究[J].光明中医,2008,23(12):1910-1913.
[12]何洋,黄敬聪,叶奕芬,等.车前草药材的质量标准研究[J].安徽农业科学,2011,39(6):3332-3333.
[13]周萍,杨月娥,杨敏.花生壳药材质量标准的研究[J].大理学院学报:综合版,2011,10(2):1-3.
[14]李盈,王举涛,刘金旗,等.HPLC法同时测定牡丹皮中芍药苷和氧化芍药苷含量[J].亚太传统医药,2016,12(21):25-27.
[15]欧金梅,吴德玲,金传山,等.HPLC法同时测定白芍总苷中4种单萜苷的含量[J].中药材,2013,36(3):423-425.
[16]何秀菊,张振秋,王婧宁,等.HPLC波长切换法同时测定桂枝、白芍药对提取物中8个成分的含量[J].药物分析杂志,2013,33(11):1899-1903.
[17]周军,张蕾,王杰.HPLC-DAD法测定脑血栓片中苦杏仁苷、羟基红花黄色素A、芍药苷、阿魏酸、丹酚酸B和丹参酮ⅡA[J].现代药物与临床,2015,30(3):262-266.
[18]严玉平,由会玲,李国川,等.芍药及不同炮制品在芍药甘草汤中芍药苷含量的差异研究[J].中国药房,2009,20(6):463-465.