提出了高效液相色谱法快速测定葡萄干中3种糠醛类物质。样品经甲醇-0.02 mol·L-1乙酸铵(用乙酸调pH 3.5)(20+80)混合溶液超声提取后,离心,取上清液过微孔滤膜过滤后供高效液相色谱分析。色谱分离采用Intersil ODS色谱柱和以不同比例的(A) 0.02 mol·L-1乙酸铵(用乙酸调pH 3.5)和(B)甲醇的混合液为流动相,对目标化合物进行梯度洗脱。流量为1.0 mL·min-1,柱温为40 ℃,检测波长为285 nm。3种糠醛的质量浓度均在0.7~500 mg·L-1范围内与相应峰面积呈线性关系,其检出限(3S/N)分别为0.4,0.5,0.3 mg·kg-1,在实样的基础上加入标准溶液进行回收试验,回收率在96.8%~109%之间,测定值的相对标准偏差(n=6)小于5%。

Three furfurals in raisins were determined by HPLC. The sample was extracted ultrasonically with a mixed solution of CH3OH and 0.02 mol·L-1 NH4OAc solution (pre-adjusted to pH 3.5 with HOAc) (20+80). The supernatant was taken for HPLC analysis. In the LC separation Intersil ODS column and mixtures of (A) solution of 0.02 mol·L-1 NH4OAc (pH 3.5) and (B) CH3OH in various ratios as mobile phase in gradient elution were adopted, with column temperature of 40 ℃ and flow-rate of the mobile phase at 1.0 mL·min-1. UV detection at 285 nm was used in common for the 3 furfurals. Linear relationships between values of peak area and mass concentration of the 3 furfurals were kept in the same range of 0.7 to 500 mg·L-1, with detection limits (3S/N) were 0.4, 0.5, 0.3 mg·kg-1 respectively. Tests for recovery were performed by addition of mixed standard solution, giving values of recovery in the range of 96.8%-109%, with RSD′s (n=6) less than 5%.