高效液相色谱-荧光法测定腊肉中的苯并芘残留
Determination of Benzo (a) pyrene in preserved ham by high performance liquid chromatography-fluorescence detection
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摘要: 建立高效液相色谱-荧光法检测腊肉中苯并芘的分析方法。以市售的腊肉作为供试样品,样品经皂化,正己烷超声提取后,用WatersXBridgeTMC18柱分离,甲醇和水(90:10,v/v)为流动相,流速为1.0mL/min,荧光检测器激发波长为365nm,检测波长为410nm,外标法峰面积定量。结果表明:苯并芘在0.002~0.5μg/mL范围内呈现良好的线性关系,相关系数0.9999,在1~10μg/kg添加水平时,加标回收率为85.14%~91.01%,相对标准偏差为1.96%~5.37%(n=6);方法的检出限和定量限分别为0.15和0.5μg/kg。该方法测定腊肉中的苯并芘方便,快捷,准确可靠,易推广使用。Abstract: The purpose was to use HPLC for the determination of the content of Benzo (a) pyrene in preserved ham.Preserved ham samples were pretreated by saponification and ultrasonic extraction, the chromatographic separation was performed on a C18 column with a mobile phase consisting of methanol and water (90:10, v/v) at 1.0mL/min.Excitation wavelength of fluorescence detector 365nm and its detection wavelength 410nm, and the quantitation method used was external standard method.Results showed that the calibration curve of the method was good linear over the range of 0.002μg/mL to 0.5μg/mL with a correlation coefficient of 0.9999.The recoveries for Benzo (a) pyrene standard spiked in the range of 1 to 10μg/kg were varied from 85.14% ~ 91.01% with a relative standard deviation (RSD) of 1.96% ~ 5.37% (n=6) .The limit of detection (LOD) and limit of quantitation (LOQ) of the developed method were 0.15 and 0.5μg/kg, respectively.The method for determination of Benzo (a) pyrene in preserved ham was convenient, fast, accurate and reliable, easy to promote the use.