中国药物警戒 ›› 2016, Vol. 13 ›› Issue (1): 16-19.

• 质量与工艺研究 • 上一篇    下一篇

苍耳子鼻炎滴丸中薄荷脑和龙脑的含量测定及指纹图谱研究

柳梦婷,方婧,唐力英,刘崇德,付梅红,吴宏伟,杨洪军   

  1. 1.中国中医科学院中药研究所 ,北京 100007;
    2.四川 禾润 制药有限公司 ,四川 资阳 641300
  • 收稿日期:2015-08-12 修回日期:2016-02-25 出版日期:2016-01-08 发布日期:2016-02-25
  • 通讯作者: 吴宏伟,男,博士,助理研究员,中药质量标准研究。
  • 作者简介:柳梦婷, 女, 硕士, 中药质量标准研究。

Determination of Menthol and Borneol and HPLC Fingerprint in Cangerzi Rhinitis Drop Pills

LIU Meng-ting1, FANG Jing1, TANG Li-ying1, LIU Chong-de2, Fu Mei-hong1, WU Hong-wei1, YANG Hong-jun1   

  1. 1. Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, China;
    2.Sichuan Herun Pharmaceutical Co., Ltd, Sichuan Ziyang 641300, China
  • Received:2015-08-12 Revised:2016-02-25 Online:2016-01-08 Published:2016-02-25

摘要: 目的 建立苍耳子鼻炎滴丸中薄荷脑和龙脑的含量测定方法及指纹图谱质量控制方法。方法 采用气相色谱法和液相色谱法分别建立苍耳子鼻炎滴丸中薄荷脑和龙脑的含量测定方法及指纹图谱质量控制方法。气相色谱法中样品采用甲醇回流法提取, 选择萘为内标物, 建立方法学。液相色谱法中样品采用乙酸乙酯提取, 300 nm 为检测波长, 甲醇-0.1% 甲酸水梯度洗脱, 建立指纹图谱质量控制方法。结果 气相色谱法中薄荷脑和龙脑的线性范围分别为0.312~0.015 6 mg·mL-1(r=0.999 9), 0.201 6~0.010 08 mg·mL-1(r=0.999 9); 平均加样回收率分别为100.99% (RSD=3.97%,n=6),97.61%(RSD=2.09%,n=6), 薄荷脑、龙脑的精密度、重复性及稳定性的RSD 均小于3%, 所检测的20 批次苍耳子鼻炎滴丸样品中薄荷脑和龙脑含量范围分别为1.34%~2.29%, 1.15%~1.61%。在色谱指纹图谱中, 共确定了19 个共有峰,利用对照品对共有峰中的3 个最高色谱峰进行了指认, 采用该方法测定20 批次样品, 除2 个批次外, 其余样品相似度均在0.95 以上。结论 所建立的含量测定及指纹图谱质量控制方法准确、可靠, 可有效地用于苍耳子鼻炎滴丸的质量控制。

关键词: 苍耳子鼻炎滴丸, 气相色谱法, 指纹图谱, 质量控制, 薄荷脑, 龙脑

Abstract: Objective To establish a method of gas chromatography and the HPLC fingerprint to evaluate the quality of Cangerzi rhinitis drop pills. Methods Using the internal standard method to analyze the content of menthol and borneol in rhinitis dripping pills by gas chromatography. Samples were extracted using methanol and the methodology was established. Ethyl acetate was applied in extracting HPLC fingerprint sample. The detected wave length was 300 nm. The separation was performed with a gradient elution composed of methanol and 0.1% formic acid-water. Results The linear range of menthol was 0.312~0.015 6 mg·mL-1, r=0.999 9, the average recovery was 100.99% (RSD=3.97%, n=6). The linear range of borneol was 0.201 6~0.010 08 mg·mL-1, r=0.999 9, the average recovery rate was 97.61% (RSD=2.09%, n=6). The RSD of precision, repeatability and stability in two components were less than 3%. The concentration of menthol and borneol in Cangerzi rhinitis dropping pills was within the range of 1.34%~2.29% and 1.15%~1.61%, respectively. In the fingerprint, 19 characteristic peaks were established, and three of that were identified. Twenty batches of Cangerzi rhinitis drop pills were determined and the similarities of 18 batches were above 0.95. Conclusion Results show that the method of gas chromatography and fingerprint is convenient,accurate and reliable,which can be applied to control the quality of Cangerzi rhinitis dripping pills.

Key words: Cangerzi rhinitis dripping pills, gas chromatography, fingerprint, quality control, menthol, borneol

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