为探究乙酰丙酮-稀释法测定白酒中甲醛含量的影响因素及贮存时间内甲醛含量的变化规律,该文以稀释法为主,纯酒样中的甲醛含量为参比,选取3个甲醛浓度的浓香型白酒为研究对象,探究测定过程中的影响因素,并通过重现性和加标回收率对该方法进行验证,最后追踪贮存时间内白酒中的甲醛含量,探究其变化规律。结果显示,乙酰丙酮-稀释法测定白酒中的甲醛含量,当甲醛含量在10 mg/L范围内,取样体积2.5 mL、水为稀释液、显色剂用量2.5 mL,于96 ℃恒温水浴中显色20 min时,该方法的检出限为 0.007 mg/L,定量限为0.021 mg/L,重现性的相对标准偏差＜5%,加标回收率在97.89%~114.91%,可满足实际样品的测定范围需求。贮存期间白酒中的甲醛含量的变化趋势相似,整体呈“前涨中缓后稳定”的趋势,但稳定时间大有不同,少则数月,多则2~3年。综上乙酰丙酮分光光度-稀释法测定白酒中甲醛含量,检出限低、重现性好,简单易操作,用时短,可用于白酒中甲醛含量的测定,在中小酒企中推广使用。
This study aimed to explore the influencing factors of formaldehyde content in Baijiu by acetylacetone spectrophotometry-diluted and the variation during storage time.In this paper, based on the dilution method, the influencing factors of formaldehyde content in Baijiu was explored by different concentrations of Baijiu as the object, referenced result before diluted.The method was verified by reproducibility and recovery rate.Finally, the formaldehyde concentration in Baijiu was tracked to explore variation during storage.Results showed when the formaldehyde content was no more than 10 mg/L,the sampling volume was 2.5 mL, water was the diluent, and the amount of solution was 2.5 mL,developing in 96 ℃ for 20 minutes the detection limit of this method was 0.007 mg/L, the limit of quantification was 0.021 mg/L, the relative standard deviation of reproducibility was<5%, and the recovery rate was 97.89%-114.91%, which met the requirements of the actual sample measurement range.The formaldehyde content in Baijiu had a similar change trend during storage, which showed was “rising in front and slowing down and then stabilizing”,but the stabilization time was very different, ranging from months to 2-3 years.The determination of formaldehyde content in Baijiu by acetylacetone spectrophotometry-dilution method had the advantages of low detection limit, good reproducibility, simple operation, and short time.It can be used for the determination of formaldehyde content in Baijiu and popularized in small and medium-sized wine enterprises.
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