腐乳中桔青霉素的测定及安全评价

Determination and safety evaluation of citrinin in sufu

中文关键词:  腐乳  桔青霉素  色谱

英文关键词:sufu  citrinin  chromatography

中文摘要:

      目的 探讨腐乳中桔青霉素的检测方法, 并对腐乳中桔青霉素的污染情况进行评估。方法 采用高效液相色谱-荧光检测法(high performance liquid chromatography-fluorescence detection, HPLC-FLD)对腐乳中桔青霉素的进行测定, 优化色谱条件及提取条件, 并对优化后的方法进行了方法学验证。结果 优化的提取条件为: 以乙腈-水(pH 2.0, 甲酸)=35:65(V:V)为流动相, 以乙腈-乙酸乙酯-甲酸(7:3:1, V:V:V)为提取液, 提取温度及提取时间分别为60 ℃和30 min。该方法在0.05~5.00 μg/mL浓度范围内的线性相关系数r2=0.9998, 回收率为91.9%~96.8%, 相对标准偏差≤3.17%。14种腐乳中有13个样品检出了桔青霉素。结论 本方法准确可靠、重现性好、灵敏度高, 可用于腐乳中桔青霉素的微量检测。

英文摘要:

      Objective To investigate the method for the determination of citrinin in sufu and evaluate the pollution situation of citrinin in sufu. Methods The citrinin in sufu was detected by high performance liquid chromatography-fluorescence detection (HPLC-FLD), the chromatographic conditions and the extracting conditions were optimized, and the optimized method was verified by methodology. Results The optimized extraction conditions were as follows: the mobile phase was acetonitrile-water (pH 2.0, formic acid, 35:65(V:V)), extracting solution was acetonitrile-ethyl acetate-formic acid (7:3:1, V:V:V), the extraction temperature and time were 60 ℃ and 30min. This method had good linear relationships in the range of 0.05~5.00 μg/mL (r2=0.9998). The recoveries were 91.9%~96.8%, with the relative standard deviations of less than 3.17%. Thirteen of the fourteen samples were detected with citrinin. Conclusion This method is accurate, reproducible and sensitive, which can be used to detect the citrinin in sufu.