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顶空气相色谱法测定厚朴中β-桉油醇含量的方法研究

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目的 研究用顶空气相色谱法测定厚朴中β-桉油醇含量的方法 .方法 采用顶空气相色谱法.色谱柱为HP-INNOWax毛细管柱,检测器为氢火焰离子化检测器,进样口温度:200℃,柱温:135℃持续3 min,以10℃/min的升温速率升至150℃,维持3 min,以15℃/min的升温速率升至250℃,持续5 min;恒定流量,流速:0.8 mL/min;检测器温度:250℃;顶空进样,气体进样量:1 mL,顶空瓶平衡温度180℃,平衡时间30 min;用外标法按峰面积计算结果 .结果 薄荷脑的检测质量浓度线性范围为2.49~24.86μg/mL(r=0.9994),精密度、稳定性、重复性试验的RSD均<5%,平均加样回收率为97.0%,RSD为0.84%(n=9).结论 该方法 用于测定挥发油类成分简便、准确.
Study on the Determination of β - Eucalyptol in Magnolia officinalis by Headspace Gas Chromatography
Objective To study the method of headspace gas chromatography for the determination of β-eugenol in Magnolia officinalis. Methods Headspace gas chromatography was used. The column was HP-INNOWax capillary column, the detector was hydrogen flame ionization detector, inlet temperature: 200 ℃; column temperature: 135 ℃ for 3min, at 10 ℃/min heating rate rose to 150 ℃, At a rate of 15 ℃/min up to 250 ℃for 5 min; constant flow rate: 0.8 mL/min; detector temperature: 250 ℃; headspace injection, gas injection volume: 1 mL, headspace Temperature 180 ℃, the balance time 30min; with the external standard method according to the peak area calculation results. Results The linear range of the concentration of menthol was 2.49~24.86 μg/mL (r=0.9994). The RSD of the precision, stability and repeatability test were <5%, the average recovery was 97.0%, RSD was 0.84% (n=9). Conclusion The method is simple and accurate for the determination of volatile oil.

headspace gas chromatographyβ-eucalyptol alcoholmagnolia

吴查青、王发英、关晓娟

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丽水市食品药品与质量技术检验检测院药品质量检测中心,浙江 丽水 323000

丽水市中心医院 药剂科,浙江 丽水 323000

顶空气相色谱法 β-桉油醇 厚朴

浙江省科技计划项目

2012C37008

2017

中国生化药物杂志
南京生物化学制药研究所,全国生化制药情报中心站,中国生化制药工业协会,中国药品生物制品检定所

中国生化药物杂志

ISSN:1005-1678
年,卷(期):2017.37(9)
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