摘要
目的建立HPLC法和液质联用法测定辣椒粉中非法添加的苏丹红。方法供试品用丙酮超声涡旋提取,采用HPLC法和液质联用法进行测定。色谱柱采用Agilent-C_(18)(100mm×4.6mm,3.5μm)柱;流动相为1mL·L^(-1)甲酸溶液-乙腈(85∶15)和1mL·L^(-1)甲酸的乙腈溶液-丙酮(80∶20);梯度洗脱;流速:1.0mL·min^(-1);检测波长:苏丹红Ⅰ478nm;苏丹红Ⅱ、Ⅲ和Ⅳ520nm;柱温:30℃。质谱条件:以三重四级杆电喷雾离子源(ESI+)扫描,干燥气体温度:300℃,干燥气体流速:3.0mL·min^(-1)。结果苏丹红Ⅰ~Ⅳ质量浓度在0~10μg·mL^(-1)范围内线性关系良好(r≥0.998);平均加样回收率均大于85%;质谱分辨率良好,方法专属性强。结论该方法操作简便、灵敏度高、结果准确、专属性强,可用于辣椒粉的质量控制。
Objective To develop a method for the determination of illegal additives sudan red in cayenne pepper by HPLC and HPLC tandem mass spectrometry.Methods Sample solutions were prepared by acetone ultrasonic vortex method.The chromatography separation was performed on an Agilent-C18 column（100 mm×4.6 mm,3.5μm）with gradient elution.The mobile phase consisted of 1 mL·L^-1 formic acid and acetonitrile at the ratio of 85∶15,and 1 mL·L^-1 formic acid acetonitrile solution with acetone（80∶20）,respectively.The detection wavelength of sudan redⅠwas 478 nm,and the detection wavelength of sudan red Ⅱ,Ⅲ,orⅣ was 520 nm.The column temperature was set at 30℃ and the flow rate was 1.0 mL·min^-1.The data was collected with triple quadruple electrospray ionization source（ESI＋）,the dry gas temperature was 300 ℃ and the flow rate of dry gas was 3.0 mL·min^-1.Results There were good linear relationships from 0 to 10μg·mL^-1 of sudan red with the correlation coefficients were all above 0.998 and the average recoveries were all above 85%.HPLC-MS has advantages of high resolution and specificity.Conclusion The proposed method is simple,sensitive,accurate and specific.Thus it can be applied to the quality control of cayenne pepper.
出处
《西北药学杂志》
CAS
2017年第6期683-686,共4页
Northwest Pharmaceutical Journal
基金
国家自然科学基金项目(编号:81573391)
