摘要:本文建立了腐竹中测定乌洛托品的方法,以乙腈提取腐竹中乌洛托品,加盐酸水解生成甲醛,以3-甲基-2-苯并噻唑啉酮腙盐酸盐水合物(酚试剂)和硫酸高铁铵与甲醛反应生成蓝绿色化合物,通过在630 nm测吸光度来间接测定乌洛托品。实验考察了盐酸的用量、水解温度、吸附剂种类、反应时间等实验条件的影响。用乙腈溶液超声10 min提取腐竹中的乌洛托品,用1.5 g中性氧化铝吸附溶液中的悬浊物,在50 ℃和0.5 ml盐酸分解得到的实验结果最佳。实验显示:脂肪、糖、蛋白质、苯丙氨酸、等对实验结果没有干扰,亚硫酸盐对实验稍有干扰。本实验线性范围在0.6~6.0 μg/ml 的范围内线性关系良好,相关系数 R2=0.9933。腐竹中的加标回收率平均88.2%。其检出限低,准确性高,稳定性好,可用于腐竹中乌洛托品的检测,相对标准偏差为1.72%。7801
关键词: 乌洛托品;腐竹;中性氧化铝;酚试剂
Determation of hexamethylenetetramine in the Fuzhu by spectrophotometry
Abstact: The thesis presents a spectrophotometric method for determing hexamethylenetetramine in fuzhu. The sample was extracted by acetonitrile. Hexamethylenetetramine is hydrolyzed into formaldehyde by hydrochloric acid. The formaldehyde can be reacted with 3-methyl-2-benzothiazolinone ketone hydrazone hydrochloride (Sawicki's Reagent) and ferric ammonium sulfate to form a blue-green compound, which can be measured by spectrophotometry at 630 nm. Some experimental conditions were investigated like the amount of hydrochloric acid, hydrolysis temperature, adsorbent, reaction time and so on. The result shows that the fat, sugar, protein, phenylalanine, did not interfere with the determination. Sulfite had some interfere. According to above experiment, 1.5 g neutral alumina was used to adsorb opaque solution, and 0.5 ml hydrochloric acid at 50 ℃ was used to hydrolyze hexamethylenetetramine. The method showed a good linearity at the range of 0.6~6.0 μg/ml for urotropine with R2=0.9933. The recoveries average 88.2%. The method was low detection limit, high accuracy, good stability which can be used for the detection of hexamethylenetetramine in fuzhu .
KeyWords: Hexamethylenetetramine;fuzhu; neutral alumina;Sawicki's Reagent