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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
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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, 0.25μm)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0.03~1.71μg/g,定量限为0.12~5.77μg/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。 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,0.25μm),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 0.03-1.71μg/g and limit of quantitation of 0.12-5.77μg/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.
作者 许恒誉 刘博 吴舜尧 乔跃辉 蔡兴华 邰胜梅 左小博 彭池方 XU Heng-Yu;LIU Bo;WU Shun-Yao;QIAO Yue-Hui;CAI Xing-Hua;TAI Sheng-Mei;ZUO Xiao-Bo;PENG Chi-Fang(Zhejiang Industrial Co.,Ltd.,China Tobacco,Ningbo 315502,China;School of Food Science and Technology,Jiangnan University,Wuxi 214122,China;Hangzhou Tea Research Institute,China COOP,Hangzhou 310016,China;Zhejiang Key Laboratory of Tea Resource Transboundary Application Technology,Hangzhou 310016,China)
出处 《食品安全质量检测学报》 2026年第1期180-186,共7页 Journal of Food Safety and Quality
基金 国家重点研发计划项目(2022YFD2101105) 浙江中烟工业有限责任公司研发项目(QG/ZY-SK-005/01x)。
关键词 有机溶剂残留 茶多酚 顶空-气相色谱法 风险分析 organic solvent residue tea polyphenols headspace-gas chromatography risk analysis
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