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目的建立高效液相色谱法测定辣椒粉和花椒粉中9种工业染料的检测方法。方法前处理方法:称取1 g样品,加一定量乙腈,摇匀,超声提取、离心,定容至20 ml,取上清液经0.45μm滤膜过滤后上机,外标法定量。色谱条件:流速1.000 ml/min;流动相:A为乙腈,B为0.02 mol/L乙酸铵及0.4%冰乙酸,pH值为4.2,梯度洗脱。进样量:10μl;柱温:40℃;检测波长为各自的最大吸收波长。结果方法的检出限为0.02~0.07 mg/kg,回收率为80.5%~111.0%,相对标准偏差为4.76%~9.05%。相关系数为0.999 5~0.999 9。结论该方法前处理简便,且能达到很好的分离效果,精密度、回收率也满足方法学要求,完全适合于对辣椒粉和花椒粉中9种工业染料进行检测。
Objective To establish a HPLC method for the determination of nine industrial dyes in paprika and pepper powder. Methods Pretreatment method: Weigh 1 g sample, add a certain amount of acetonitrile, shake, ultrasonic extraction, centrifugation, constant volume to 20 ml, the supernatant was filtered through 0.45μm membrane on the machine, external standard. Chromatographic conditions: flow rate 1.000 ml / min; mobile phase: A acetonitrile, B 0.02 mol / L ammonium acetate and 0.4% glacial acetic acid, pH 4.2, gradient elution. Injection volume: 10μl; column temperature: 40 ℃; detection wavelength for the respective maximum absorption wavelength. Results The detection limit was 0.02 ~ 0.07 mg / kg, the recoveries were 80.5% ~ 111.0%, and the relative standard deviations were 4.76% ~ 9.05%. The correlation coefficient is 0.999 5 ~ 0.999 9. Conclusion The pretreatment method is simple, and can achieve good separation effect. The precision and the recovery rate also meet the methodological requirements. It is suitable for the detection of nine industrial dyes in paprika and pepper powder.