提出了连续流动注射分光光度法同时测定杏仁中氰化物和挥发酚含量的方法。2.00 g杏仁样品经25 mL 0.05 mol·L^-1硫酸溶液涡旋1 min,浸泡10 min,水解释放样品中氰苷后,用2 g·L^-1氢氧化钠溶液固定待测物,并定容至50 mL。取上清液,经0.45 μm滤膜过滤,滤液在优化的试验条件下采用连续流动注射分光光度法测定其中氰化物和挥发酚的含量。结果表明,氰化物和挥发酚的质量浓度在0.002~0.200 mg·L^-1内与对应的峰高呈线性关系,检出限分别为0.005 mg·kg^-1和0.017 5 mg·kg^-1。取3份样品,每个样品重复测定6次,测定值的相对标准偏差(n=6)均小于2.0%。按照标准加入法对实际样品进行回收试验,回收率为97.6%~105%。方法用于分析10份杏仁样品,氰化物的检出量为10.6~56.4 mg·kg^-1,平均值为32.3 mg·kg^-1,挥发酚的检出量为14.7~54.8 mg·kg^-1,平均值为31.9 mg·kg^-1。方法利用硫酸溶液水解样品中氰苷后用碱溶液固定,解决了碱溶液直接提取结果偏低的问题。

A method for simultaneous determination of cyanide and volatile phenol in almond by continuous flow injection spectrophotometry was proposed. The almond sample (2.00 g) was whirled for 1 min and soaked for 10 min in 25 mL of 0.05 mol·L^-1 sulfuric acid solution. After hydrolyzed to release cyanide glycosides in the sample, 2 g·L^-1 sodium hydroxide solution was added to fix the test substance and make its volume up to 50 mL. The supernatant was taken and passed through 0.45 μm filter membrane, in which cyanide and volatile phenol was determined by continuous flow injection spectrophotometry under optimized experimental conditions. As shown by the results, linear relationships between values of the corresponding peak height and mass concentration of cyanide and volatile phenol were found in the range of 0.002-0.200 mg·L^-1, with detection limits of 0.005 mg·kg^-1 for cyanide, 0.017 5 mg·kg^-1 for volatile phenol, respectively. The 3 samples were taken and determined 6 times repeatedly for each sample, with RSDs (n=6) of the determined values less than 2.0%. Test for recovery was made on the actual samples by the standard addition method, giving results in the range of 97.6%-105%. This method was applied to analysis of 10 almond samples, and the detection amounts of cyanide were 10.6-56.4 mg·kg^-1, with an average value of 32.3 mg·kg^-1, while the detection amounts of volatile phenol were 14.7-54.8 mg·kg^-1, with an average value of 31.9 mg·kg^-1. In this method, sulfuric acid solution was used to hydrolyze the cyanide glycoside in the sample and then it was fixed with alkaline solution, which could solve the problem of low results obtained by direct extraction with alkaline solution.