宁夏医科大学学报2024,Vol.46Issue(10) :1069-1073.DOI:10.16050/j.cnki.issn1674-6309.2024.10.017

麝香止痛贴膏挥发性成分测定及质量评价

Determination and Quality Evaluation of Volatile Components in Shexiang Zhitong Plaster

董文静 李鹏飞 张美 张宇欣 李哲 王庆
宁夏医科大学学报2024,Vol.46Issue(10) :1069-1073.DOI:10.16050/j.cnki.issn1674-6309.2024.10.017

麝香止痛贴膏挥发性成分测定及质量评价

Determination and Quality Evaluation of Volatile Components in Shexiang Zhitong Plaster

董文静 1李鹏飞 1张美 1张宇欣 1李哲 2王庆1
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作者信息

  • 1. 宁夏回族自治区药品检验研究院,宁夏回族自治区药品质量控制与评价重点实验室,宁夏回族自治区药品监督管理局中药质量控制重点实验室,银川 750001
  • 2. 宁夏医科大学药学院,银川 750004
  • 折叠

摘要

目的 建立以萘为内标,麝香止痛贴膏中薄荷脑、冰片、水杨酸甲酯的气相含量测定法.方法 采用DB-WAX毛细管柱(30 m × 0.32 mm,0.5 μm)、氢火焰离子化检测器(FID),色谱柱初始温度为100 ℃,以4 ℃·min-1的速率升至200 ℃,保持6 min,流速1.8 mL·min-1,分流比10:1,进样量1.0 μL.结果 薄荷脑、冰片、水杨酸甲酯分别在 0.099 8~0.598 6 g·L-1(r=0.999 8)、0.126 8~0.760 7 g·L-1(r=0.999 7)、0.103 9~0.623 6 g·L-1(r=0.999 8)范围内线性关系良好,平均回收率分别为102.1%、98.5%、100.8%,RSD分别为1.9%、1.9%、1.6%.经测定9个厂家的样品后发现,各厂家间的挥发性成分含量差异较大,热压法工艺对挥发性成分含量的影响小于溶剂法.结论 本方法操作简单、准确,重复性、稳定性良好,可为麝香止痛贴膏质量提升提供科学依据.

Abstract

Objective To establish a gas chromatography method for the simultaneous determination of menthol,borneol and methyl salicylate in Shexiang Zhitong plaster with naphthalene as an internal standard.Methods A DB-WAX capillary column(30 m × 0.32 mm,0.5 μm)and a FID detector were used.The initial temperature was 100℃,and the temperature was raised to 200 ℃ at the rate of 4 ℃ min-1,maintained for 6 min.The flow rate was 1.8 mL·min-1,the split ratio was 10:1,and the injection volume was 1.0 μL.Results Menthol,bornol and methyl salicylate were linear in the range of 0.099 8-0.598 6 g·L-1(r=0.999 8),0.126 8-0.760 7 g·L-1(r=0.999 7)and 0.103 9-0.623 6 g·L-1(r=0.999 8).The average recoveries were 102.1%,98.5%and 100.8%respectively.RSD was 1.9%,1.9%and 1.6%respectively.After determining the samples from 9 manufacturers,it was found that there were significant differences in the content of volatile components among different manufacturers,and the influence of the hot pressing process on the content of volatile components was less than that of the solvent method.Conclusion The method is simple,accurate,repeatable and stable,which can provide a scientific basis for the quality control of Shexiang Zhitong plaster.

关键词

麝香止痛贴膏/含量测定/内标法/挥发性成分/超声提取法

Key words

Shexiang Zhitong plaster/content determination/internal standard method/volatile components/ultrasonic extraction method

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出版年

2024
宁夏医科大学学报
宁夏医科大学

宁夏医科大学学报

CSTPCD
影响因子:0.84
ISSN:1674-6309
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