亲水性色谱柱高效液相色谱法测定米面及制品中的乌洛托品

Determination of methenamine in rice, flour and their products by hydrophilic chromatographic column high performance liquid chromatography

中文关键词:  乌洛托品  亲水性色谱柱  高效液相色谱法  米面制品

英文关键词:methenamine  hydrophilic chromatographic columnrice  high performance liquid chromatography  rice, flour and their products

中文摘要:

      目的 建立亲水性色谱柱高效液相色谱法(high performance liquid chromatography, HPLC)检测米面及制品中乌洛托品的方法。方法 样品中的乌洛托品以20 mmol/L乙酸铵溶液(氨水, pH 10)为提取液, 超声提取10 min, 10000 r/min离心3 min后取上清液过0.22 μm水相微孔滤膜待测。对50.00 mg/L的乌洛托品标准溶液色谱峰进行光谱扫描, 确定乌洛托品的最大吸收波长为210 nm。采用Waters XBridge BEH HILIC (4.6 mm×150 mm, 3.5 μm), 色谱柱进行分离, 以纯水:乙腈=70:30(V:V)为流动相, 外标法定量。结果 乌洛托 品在0~200 mg/L范围内具有良好的线性关系, 其线性方程为Y=1.647X+0.3669, 相关系数为0.9999, 方法检出限为4.00 mg/kg。在4.00、8.00、40.00 mg/kg 3个水平下的回收率分别为93.5%、96.4%、98.7%, 相对标准偏差分别为4.2%、3.2%、1.5%。结论 该方法符合GB/T27404-2008《实验室质量控制规范食品理化检测》的相应技术要求, 方法准确稳定可靠, 适合测定米面及制品中的乌洛托品。

英文摘要:

      Objective To establish a method for determination of methenamine in rice, flour and their products by hydrophilic chromatographic column high performance liquid chromatography. Methods The methenamine in the sample was extracted with 20 mmol/L ammonium acetate solution (ammonia water, pH 10) by ultrasonic for 10 min, centrifuged at 10000 r/min for 3 min, and then the supernatant was filtered through 0.22 μm aqueous micropores. A spectral scan of 50.00 mg/L urotropine standard solution was carried out and the maximum absorption wavelength of urotropine was 210 nm. The sample was separated by Waters XBridge BEH HILIC (4.6 mm×150 mm, 3.5 μm) with pure water: acetonitrile=70:30 (V:V) as mobile phase, and quantified by external standard solution.Results Methenamine had a good linear relationship in the range of 0-200 mg/L, the linear equation was Y=1.647X+0.3669, the correlation coefficient was 0.9999 and the limit of detection was 4.00 mg/kg. The recoveries at 3 levels of 4.00, 8.00, and 40.00 mg/kg were 93.5%, 96.4% and 98.7%, respectively, and the relative standard deviations were 4.2%, 3.2%, and 1.5%, respectively. Conclusion This method meets the technical requirements of GB/T27404-2008 Laboratory Quality Control Specification Food Physical and Chemical Testing, and it is accurate, stable and reliable, which is suitable for determination of methenamine in rice, flour and their products.