低温离心净化-高效液相色谱法快速测定腐竹中的碱性橙II和碱性嫩黄O

Rapid determination of chrysoidine II and auramine O in dried bean curd sticks by cryogenic centrifugal purification–high performance liquid chromatography

目的建立腐竹中碱性橙II和碱性嫩黄O的低温离心净化-高效液相色谱测定方法。方法样品经70%的乙腈-氨水(0.5%)提取,4℃低温、12000 r/min离心净化,高效液相色谱(high performance liquid chromatography,HPLC)分离,最后采用二极管阵列检测器(PDA)检测,以保留时间(Rt)定性,外标法定量。结果在0.00125~0.05 mg/m L的浓度范围内,标准曲线有良好的线性关系,相关系数大于0.9999;样品在0.05、2.0、10.0 mg/kg三个加标水平内的回收率范围为95.0%~103.0%(n=10),相对标准偏差小于5.0%。方法的检出限(LOD)为0.02 mg/kg,定量限(LOQ)为0.05 mg/kg。结论对实际样品测试结果与参考文献方法比较,该方法具有简便、快速、灵敏、费用低,便于推广应用。

ABSTRACT:Objective Toestablish a method to detect chrysoidine II and auramine O in dried bean curd sticks by cryogenic centrifugal purification–high performance liquid chromatography. Methods The samples werediluted and extracted by 70% acetonitrile ammonia water, purified by centrifugation at 12000 r/min and 4℃, separated by high performance liquid chromatography (HPLC), and detected by photodiode array detector (PDA). The method took the retention time (Rt) for qualitative and external standard method quantitative analysis.Results Within the limits of concentration 0.00125~0.05 mg/mL, the standard curve had a good linear relationship, and the correlation coefficient was more than 0.9999; in the level of 0.05, 2.0, and 10.0 mg/kg, the add mark recovery rate was from 95.0% to 103.0%(n=10), the relative standard deviation was less than 5.0%; limit of detection(LOD) was 0.02 mg/kg, limit of quantitation (LOQ) was 0.05 mg/kg.Conclusion Comparing the actual sample testing results with reference method, this method is simple, rapid, sensitive, with low cost, and is suitable for popularization and application.