摘要
目的:建立高效液相色谱法同时测定小麦粉中4种禁用成分(曲酸、噻二唑、间苯二酚和硫脲)。方法:样品采用体积分数70%的乙醇提取,经超声、离心、蒸干,流动相复溶处理,采用Shim-pack VP-ODS C18色谱柱,以2 g/L的乙酸溶液和甲醇(70∶30,V/V)为流动相,流速为1.0 mL/min,柱温为30 ℃,二极管阵列检测器(DAD)进行检测,检测波长为240、275和300 nm,外标法定量。结果:4种化合物在1.0~100 mg/L范围内线性关系良好,相关系数(r2)均大于0.999,方法的检出限(以信噪比为3计)为0.5 μg/g(噻二唑、硫脲)、1.0 μg/g(曲酸、间苯二酚),加标水平为5倍检出限(LOD)~10倍LOD时加标回收率为98.0%~99.7%,RSD均小于1.0%。结论:该方法前处理简单,回收率高,精密度好,适用于小麦粉中4种禁用成分的定性定量检测。
Objective:Using high performance liquid chromatography to simultaneously determine four kinds of prohibited components in wheat flour including kojic acid, 2-mercapto-5-methyl-1,3,4-thiadiazole, resorcinol and thiourea. Methods: Samples were extracted directly with φ(COMHIOH)=70% ethanol. The sample solution was ultrasonic, centrifuged at a speed of 6 000 r/min, steamed and dissolved in mobile phase. The solution was analyzed on an Shim-pack VP-ODS C18 column (250 mm×4.6 mm, i.d 5 μm) using 2 g/L acetic acid-thanol(70:30, V/V)as mobile phase at a flow rate of 1.0 mL/min. The temperature of the column was set at 30 ℃. The detection wavelengths were 240 nm, 275 nm and 300 nm. Results: The standard working curves of 4 compounds had good linear relationships (r2>0.999) in concentration range of 1.0~100 mg/L. The detection limits (S/N=3) of 4 compounds were 0.5 μg/g (2-mercapto-5-methyl-1,3,4-thiadiazole, thiourea) and 1.0 μg/g (kojic acid and resorcinol). The recoveries of 4 analytes at spiked levels of 5 times LOD-10 times LOD were in the range of 98.0%~99.7% with relative standard deviations less than 1.0%. Conclusion: With the advantages of simplicity, high recovery and good precision, this method is suitable for the determination of 4 prohibited components in flour.
作者
申科敏
胡晓琴
郭崇政
Shen Kemin;Hu Xiaoqin;Guo Chongzheng(Department of Public Health and Preventive Medicine, Changzhi Medical College)
出处
《长治医学院学报》
2019年第2期98-101,共4页
Journal of Changzhi Medical College
关键词
小麦粉
曲酸
噻二唑
间苯二酚
硫脲
高效液相色谱法
wheat flour
kojic acid
2-mercapto-5-methyl-1,3,4-thiadiazole
resorcinol
thiourea
high performance liquid chromatography (HPLC)