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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。
OBJECTIVE To establish a method for the determination of basic orange II and alkaline yellow O in Yuba by low temperature centrifugation and high performance liquid chromatography. Methods The samples were extracted with 70% acetonitrile-ammonia (0.5%), centrifuged at 12000 r / min at 4 ℃, and separated by high performance liquid chromatography (HPLC). Finally, the detection was performed by using a diode array detector , With retention time (Rt) qualitative, external standard method. Results The calibration curve showed a good linearity in the concentration range of 0.00125 ~ 0.05 mg / mL with the correlation coefficient greater than 0.9999. The recoveries of the samples in three spiked levels of 0.05, 2.0, 10.0 mg / kg were 95.0% ~ 103.0% (n = 10), the relative standard deviation is less than 5.0%. The limit of detection (LOD) was 0.02 mg / kg and the limit of quantitation (LOQ) was 0.05 mg / kg. Conclusion Compared with the reference methods, this method is simple, rapid, sensitive, low cost and easy to popularize.