葡萄酒中12种农药残留分析及膳食风险评估  

Analysis and dietary risk assessment of 12 pesticide residues in wine

作　　者：汤丽华 朱燕燕 郭阳 吕毅 TANG Lihua;ZHU Yanyan;GUO Yang;LV Yi(Key Laboratory of Quality and Safety of Wolfberry and Wine for State Administration for Market Regulation,Ningxia Food Testing and Research Institute,Yinchuan 750001,China)

机构地区：[1]宁夏回族自治区食品检测研究院(国家市场监管重点实验室(枸杞及葡萄酒质量安全)),宁夏银川750001

出　　处：《中国酿造》2025年第3期272-278,共7页China Brewing

基　　金：国家市场监管总局科技计划项目(2022MK129);宁夏回族自治区重点研发项目(2022BEG03170)。

摘　　要：利用高效液相色谱-串联质谱法(HPLC-MS/MS)对葡萄酒中335种农药进行初筛,筛选出检出率较高的霜霉威等12种农药,采用QuEChERS-HPLC-MS/MS对其建立测定方法,并对其膳食风险进行评估。结果表明,采用乙腈提取,QuEChERS法净化,在电喷雾正离子(ESI+)模式下电离,使用多反应监测(MRM)模式对各农药进行测定,并用基质匹配标准溶液外标法进行定量分析。12种农药在1~200 ng/mL质量浓度范围内线性关系良好,相关系数R均>0.997,方法检出限(LOD)、定量限(LOQ)分别为0.0005 mg/kg、0.001 mg/kg,平均加标回收率为82%~110%,精密度试验结果的相对标准偏差(RSD)为2.5%~9.2%。膳食风险评估结果表明,我国不同人群11种农药的慢性风险熵(RQc)范围为1.2×10^(-6)~1.1×10^(-3),5种农药的急性风险熵(RQa)范围为9.2×10^(-6)~2.5×10^(-3),表明葡萄酒中霜霉威、啶虫脒、多菌灵、甲基硫菌灵和烯酰吗啉等农药残留不会对消费者造成不可接受的风险。335 pesticides in wine were preliminarily screened by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),12 pesticides with high detection rate,such as propamocarb were selected and determined by QuEChERS-HPLC-MS/MS,and their dietary risk was evaluated.The results showed that each pesticide was extracted by acetonitrile,purified by QuEChERS method,ionized by electrospray ionization positive ions(ESI+)mode,determined by multiple reaction monitoring(MRM)mode,and quantitatively analyzed by matrix matching standard solution external standard method.The linear relationships of 12 pesticides were good in the mass concentration range of 1-200 ng/ml,and the correlation coefficients R were all greater than 0.997.The limits of detection(LOD)and limits of quantitation(LOQ)were 0.0005 mg/kg and 0.001 mg/kg,respectively.The average standard recovery rates were 82%-110%.The relative standard deviation(RSD)of the precision tests was 2.5%-9.2%.The results of dietary risk assessment showed that the chronic risk entropy(RQc)of 11 pesticides were 1.2×10^(-6)-1.1×10^(-3),and the acute risk entropy(RQa)of 5 pesticides were 9.2×10^(-6)-2.5×10^(-3),indicating that the pesticide residues such as propamocarb,acetamiprid,carbendazim,thiophanate methyl and dimethomorph in wine did not pose an unacceptable risk to consumers.

关 键 词：高效液相色谱-串联质谱法 QUECHERS 葡萄酒 农药残留 膳食风险评估 

分 类 号：TS262.6[轻工技术与工程—发酵工程]