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
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。
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.
标题：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
英文标题：Determination of methenamine in rice, flour and their products by hydrophilic chromatographic column high performance liquid chromatography
作者：
彭名军 广州市食品检验所
宋安华 广州市食品检验所
黄儒强 华南师范大学
吴嘉文 广州市食品检验所
曾豪威 广州市食品检验所
曹霞飞 广州市食品检验所
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,
发表日期：2018-06-15
- 文件大小:
- 7.44 MB
- 下载次数:
- 60
-
高速下载
|
