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顶空气相色谱法测定虾青素中甲醇和乙醇的残留量

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(目的)建立顶空气相色谱法测定虾青素中甲醇和乙醇残留量的检测方法.(方法)采用顶空气相色谱法(FID检测器),加热箱温度60 ℃,定量环/阀温度70 ℃,传输线温度80℃,样品瓶平衡时间10.0 min,进样持续时间1.0 min,GC循环时间30.0 min,DB-624 UI(30 m×0.32 mm × 1.8 μm)色谱柱,程序升温,载气为氮气,进样口温度200 ℃,检测器温度230℃.(结果)甲醇和乙醇分离度良好,甲醇在0.05~0.5 mg/mL的范围内线性良好,平均回收率为97.7%(RSD为0.72%);乙醇在0.05~0.5 mg/mL的范围内线性良好,平均回收率为97.9%(RSD为0.97%).(结论)经方法学验证,通过实验建立的方法简单、快捷、灵敏度高和重现性好,适用于虾青素中的残留溶剂检测及确证.
Study on the Detection Method of the Residual Solvent in Astaxanthin
(Objective)To establish a detection method for measuring methanol and ethanol residues in Astaxanthin by Headspace gas chroma-tography.(Methods)Headspace gas chromatography(Flame Ionization Detector),heating box temperature 60 ℃,quantitative ring/valve temperature 70 ℃,transmission line temperature 80℃,sample bottle balance time 10.0 minutes,injection duration 1.0 minutes,and GC cy-cle time 30.0 minutes.DB-624 UI(30m×0.32 mm 1.8 μ m)capillary column,the load gas is nitrogen,inlet temperature 200 ℃,detector temperature 230 ℃.(Results)Methanol and Ethanol were well separated,Methanol was linearly in the concentration range of 0.05 mg/mL~0.5 mg/mL.There was good linear relationship,the average recovery was 97.7%(RSD 0.72%);Ethanol was linearly in the concentration range of 0.05 mg/mL~0.5 mg/mL,There was good linear relationship,the average recovery was97.9%(RSD 0.97%).(Conclusion)This method has simple,rapid,high sensitivity and good reproducibility,Is can be used for detection and confirmation of residual solvent in Astaxan-thin.

AstaxanthinMethanolEthanolResidual SolventHeadspace Gas Chromatography

农利、李丽波、严靖婷、胡倩、杨鹏、张娇、杨少杰

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云南现代民族药工程技术研究中心,云南 昆明 650501

云南省科学技术院生物医药中心,云南 昆明 650051

虾青素 甲醇 乙醇 残留溶剂 顶空气相色谱法

2024

云南化工
云南省化工研究院 云天化集团有限责任公司 云南煤化工集团有限公司 云南省化学化工学会

云南化工

影响因子:0.272
ISSN:1004-275X
年,卷(期):2024.51(10)