肉苁蓉和西洋参的乙醇提取液及回收乙醇中5种农药残留转移规律研究

Study on the transfer behavior of 5 kinds of pesticide residues in ethanol extracts and recycled ethanol of Cistanche deserticola and American Ginseng

目的研究肉苁蓉和西洋参在乙醇提取及回收乙醇过程中的农药转移规律。方法以肉苁蓉和西洋参混合样品为原料,采用超高效液相色谱-串联质谱法评估5种典型农药从原料乙醇提取到回收乙醇过程中的转移情况;同时通过气相色谱-串联质谱法研究了回收乙醇中挥发性组分残留及转移情况,通过紫外吸光度扫描和高效液相色谱法对不挥发性杂质进行了分析。结果农药强化样品在乙醇提取及后续回收乙醇过程,乙醇提取液中5种农药残留量整体上从高到低依次为治螟磷>啶虫脒>克百威>多菌灵>甲拌磷,但是仅有治螟磷转移至回收乙醇。随乙醇使用次数增加,加工因子(processing factor,PF)增大。回收乙醇在240、250~260和270~340 nm的吸光度值均超出了《中国药典》对乙醇的要求值。结论大部分农药都可转移至乙醇提取液;回收乙醇循环使用18次内,检出挥发性组分和非挥发性组分残留且随乙醇使用次数增加,不断转移累积。本研究将有助于回收乙醇的安全性监测,以及预测其是否能交叉应用于其他类型保健食品原料功能因子的提取。

Objective To evaluate the pesticide transfer behavior of Cistanche deserticola and American ginseng during the ethanol extraction and ethanol recovery process.Methods In this study,a pesticide-enhanced combinated samples of Cistanche deserticola and American Ginseng were utilized as the raw materials.Ultra performance liquid chromatography-tandem mass spectrometry was employed to assess the transfer of 5 typical pesticides from the raw ethanol extraction to the recycled ethanol.Simultaneously,the volatile components residues in the recycled ethanol were analyzed using gas chromatography-tandem mass spectrometry.Non-volatile impurities were investigated through ultraviolet absorbance scanning and high performance liquid chromatography.Results In the process of ethanol extraction and subsequent ethanol recovery of pesticide enhanced samples,the residues of 5 kinds of pesticides in the ethanol extract were in the order from high to low as chlorphos>chloramidine>carbovir>carbendazim>methylphos,but only chlorphos was transferred to recycled ethanol.The processing factor(PF)increased with each ethanol use.The absorbance values of recycled ethanol at 240,250–260,and 270–340 nm all exceed the requirements for ethanol in the Chinese pharmacopoeia.Conclusion Most pesticides transferred to ethanol extractions.Both volatile residues and non-volatile residues accumulated with the number of ethanol uses with 18 recycling cycles.This research will support the safety surveillance of recycled ethanol and forecast its potential for cross-application in extracting functional components from medicinal and edible ingredients.