顶空-气相色谱法测定茶多酚中7种有机溶剂残留及其风险分析

Determination of 7 kinds of organic solvent residues in tea polyphenols by headspace-gas chromatography and its risk analysis

中文关键词:  有机溶剂残留  茶多酚  顶空-气相色谱法  风险分析

英文关键词:organic solvent residue  tea polyphenols  headspace-gas chromatography  risk analysis

中文摘要:

      目的 建立顶空-气相色谱法(headspace-gas chromatography, HS-GC)测定茶多酚中7种有机溶剂残留并进行风险分析。方法 以50% N,N-二甲基乙酰胺溶液为基质, 经DB-23毛细管柱(60 m×0.32 mm, 0.25 μm)分离, 氢火焰离子化检测器(flame ionization detector, FID)检测, 建立了同时测定茶多酚中7种有机溶剂残留(正己烷、甲醇、二氯甲烷、丙酮、乙醇、三氯甲烷和乙酸乙酯)的分析方法。结果 HS-GC可以将7种待测溶剂很好地进行分离, 其日内精密度和日间精密度良好。标准曲线在所考察的浓度范围内呈良好的线性关系, 检出限为0.03~1.71 μg/g, 定量限为0.12~5.77 μg/g。同时, 对市场上27批茶多酚样品进行残留检测和风险分析发现, 参照《中国药典》规定, 部分茶多酚样品中检出甲醇、乙酸乙酯、正己烷和乙醇, 其中有33.33%样品的正己烷和14.81%样品的乙醇超标, 但通过每日允许暴露量(permissible daily exposure, PDE)分析, 正己烷和乙醇带来的健康风险较低。结论 本研究方法简便、准确, 可用于茶多酚中7种有机溶剂残留的测定。

英文摘要:

      Objective To establish a method for the determination of 7 kinds of organic solvent residues in tea polyphenols by headspace-gas chromatography (HS-GC), and conduct risk analysis. Methods A method for simultaneous determination of 7 kinds of organic solvent residues (n-hexane, methanol, dichloromethane, acetone, ethanol, trichloromethane and ethyl acetate) in tea polyphenols was established using a 50% N,N-dimethylacetamide solution as the matrix, separated by a DB-23 capillary column (60 m×0.32 mm, 0.25 μm), and detected by a flame ionization detector (FID). Results HS-GC could effectively separate 7 kinds of solvents to be tested, with good intra day and inter day precision. The standard curve showed a good linear relationship within the concentration range under investigation, with limit of detection of 0.03–1.71 μg/g and limit of quantitation of 0.12–5.77 μg/g. At the same time, residue testing and risk analysis were conducted on 27 batches of tea polyphenol samples in the market. According to the regulations of Chinese Pharmacopoeia, methanol, ethyl acetate, n-hexane and ethanol were detected in some tea polyphenol samples. Among them, 33.33% of the samples had n-hexane and 14.81% of the samples had ethanol exceeding the standard. However, through the analysis of permissible daily exposure (PDE), the health risks caused by n-hexane and ethanol were relatively low. Conclusion This research method is simple, accurate, and suitable for the determination of 7 kinds of residual organic solvents in tea polyphenols.