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机构地区:[1]镇江市疾病预防控制中心,江苏镇江212004
出 处:《中国卫生检验杂志》2017年第21期3077-3079,3101,共4页Chinese Journal of Health Laboratory Technology
摘 要:目的建立高效液相色谱法同时测定薯片中罗丹明B、碱性橙2、碱性橙21、碱性橙22、酸性橙Ⅱ、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ9种非法添加的工业染料。方法样品用丙酮-水(95∶5,V/V)混合溶液超声提取定容至10 ml,使用ZORBAX Eclipse Plus-C_(18)色谱柱(4.6 mm×250 mm,5μm),20 mmol/L乙酸铵水溶液(含0.1%甲酸)-甲醇为流动相,流速为1.0 ml/min,采用梯度洗脱,二极管阵列检测器测定,以保留时间定性,外标法峰面积定量。结果9种目标化合物在实验条件下能完全分离,在0.1μg/ml^5.0μg/ml内呈现良好的线性关系,相关系数均>0.999,检出限为0.05 mg/kg^0.25 mg/kg,3种浓度的加标回收率为80.2%~93.0%,相对标准偏差在2.8%~6.0%。结论本方法经实际应用证明,前处理过程简单,且准确度和精密度满足方法学要求,可应用于薯片中9种工业染料的实验室快速检测。Objective To develop a method for the determination of 9 illegally added industrial dyes( Rhodamine B,Basic Orange 2,Basic Orange 21,Basic Orange 22,Acid Orange Ⅱ,Sudan Ⅱ,Sudan Ⅱ,Sudan Ⅲ,Sudan Ⅳ) in chips by high performance liquid chromatography( HPLC). Methods The samples were mixed with acetone-water( 95 ∶5,V/V),and treated by ultrasonic extraction,then set the volume to 10 ml. Separations were performed with ZORBAX Eclipse Plus-C18 column( 4. 6 mm × 250 mm,5 μm) and gradient eluted of 20 mmol/L ammonium acetate aqueous solution( containing 0. 1% formic acid)-methyl alcohol at a flow rate of 1. 0 ml/min. Diode array detector( DAD) was used to detect the concentrations of industrial dyes,which were qualitatively determined by retention time and quantitatively determined by peak area of external standard calibration. Results 9 industrial dyes could be completely separated under the condition of HPLC. The linear ranges were within 0. 1 μg/ml-5. 0 μg/ml,and the relative coefficients( r) were greater than 0. 999. The detection limits of industrial dyes was within 0. 05 mg/kg-0. 25 mg/kg. The average recoveries of adding standard at three levels and relative standard deviations( RSDs) were within 80. 2%-93. 0% and 2. 8%-6. 0%,respectively. Conclusion It is proved by practical application that the pretreatment of this method is simple. The precision and recovery rate can meet the methodological requirements.The method can be used in the laboratory for the rapid detection of industrial dyes in chips.
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