Werkhoff P, Bretschneider W
Z Lebensm Unters Forsch. 1986 Apr;182(4):298-302. doi: 10.1007/BF01027628.
A gas chromatographic method for the quantitative determination of diethylene glycol in wine, red and white grape juice, and red and white grape juice concentrates is described. The method includes continuous extraction of the diethylene glycol with ethyl acetate by the aid of a rotation perforator. Using the new generation of chemically bonded stationary phases on fused silica together with an appropriate modern cold on-column injection system coupled with an autoanalyzer and a retention gap, the GLC analysis is shown to provide adequate information for quality control purposes. Linearity, precision and recovery with the described procedure were investigated. The precision of the method was studied using a sample containing approximately 65 mg/l diethylene glycol. Twelve separate determinations were performed by the described method; the coefficient of variation was 3.9%. The detection limit of our method is 5 mg/l diethylene glycol both for wine, grape juice and grape juice concentrates. Recovery data are based on wine, grape juice and grape juice concentrates fortified with diethylene glycol at different levels. The ranges of concentration used in this study were 10 mg/l to 10 g/l for wine and 10 mg/l to 100 mg/l for grape juice and grape juice concentrate. The average recovery of diethylene glycol for wine at all concentrations tested was 98.8%; coefficients of variation were between 1.6 and 8.0%. Recoveries of diethylene glycol added to grape juice at the level of 10 mg/l to 100 mg/l were 96% to 109%.
描述了一种气相色谱法,用于定量测定葡萄酒、红葡萄汁、白葡萄汁以及红葡萄汁浓缩物和白葡萄汁浓缩物中的二甘醇。该方法包括借助旋转穿孔器用乙酸乙酯连续萃取二甘醇。使用新一代的熔融石英化学键合固定相,结合适当的现代冷柱头进样系统、自动分析仪和保留间隙,气相色谱分析显示可为质量控制目的提供充分信息。研究了所述程序的线性、精密度和回收率。使用含有约65mg/l二甘醇的样品研究了该方法的精密度。通过所述方法进行了12次独立测定;变异系数为3.9%。我们的方法对葡萄酒、葡萄汁和葡萄汁浓缩物中二甘醇的检测限均为5mg/l。回收率数据基于用不同水平二甘醇强化的葡萄酒、葡萄汁和葡萄汁浓缩物。本研究中使用的浓度范围对于葡萄酒为10mg/l至10g/l,对于葡萄汁和葡萄汁浓缩物为10mg/l至100mg/l。在所有测试浓度下,葡萄酒中二甘醇的平均回收率为98.8%;变异系数在1.6%至8.0%之间。添加到葡萄汁中浓度为10mg/l至100mg/l的二甘醇的回收率为96%至109%。