【摘要】 建立了以橘红2号为内标物,采用高效液相色谱法测定辣椒制品中苏丹红的方法。样品经乙腈提取、超声30min后过滤。滤液加入氯化钠置于分液漏斗中振荡静置分层。蒸发溶剂至干后加入10m L乙腈溶解。用6m L甲醇洗活化后的氨基固相萃取小柱净化待测溶液。采用Nova-Pak C18色谱柱(3.9mm×15mm×5μm)分离,以乙腈(A)、超纯水(B)为流动相梯度洗脱:0~3min A70%、B30%;3~4.5min A70%~95%、B30%~5%;4.5~7.5min A95%、B5%;7.5~8.5min A95%~70%、B5%~30%。流速0.3m L/min,检测波长515nm。结果表明,在该条件下橘红2号与样品中的苏丹红分离完全,可以作为测定苏丹红的内标物。在添加浓度0.5~1.5mg/kg范围内,4种苏丹红色素的回收率在88.7%~99.7%之间,相对标准偏差(RSD)<0.25%,最低检出限(信噪比S/N=3)分别为0.56、0.53、046、0.33μg/kg。该方法操作简单、准确性好,具有良好的稳定性和重现性,可用于辣椒制品中苏丹红含量分析。更多还原

【Abstract】 Orange 2 was chosen as the internal standard substance in determination of Sudan red in chili products by HPLC. Sample was extracted by acetonitrile then ultrasonic 30 min and filtering. The filtrate was mixed with sodium chloride and set in funnel and stood for stratification. After solvent evaporated,10 ml acetonitrile solution was then added. Then 6 ml methanol was used to wash activated and small column purified amino solid phase extraction. The Nova- Pak C18 chromatographic column(3.9mm * 15 mm * 5(including m)was used in separation with mobile phase acetonitrile(A),ultrapure water(B)gradient elution :0 ~ 3 min,B30 A70% %;3 ~ 4.5min A70% ~ 95% and B30% ~ 5%;4.5 ~ 7.5min A95,B5% %;7.5 ~ 8.5min A95 % ~ 70% and B5 % ~ 30%. The flow rate was 0.3 m L/min,detection wavelength was 515 nm. The results showed that under the above conditions,Orange 2 was completely separated from the Sudan red in the samples which can be used as the internal standard determination of Sudan red. In the range of 0.5 ~ 1.5 mg/kg,the recovery rate of 4 kinds of Sudan red pigment was between 88.7% ~ 99.7%,relative standard deviation(RSD)< 0.25%,the lowest detection limit signal-to-noise ratios(S/N = 3)were 0.56,0.53,046,0.33g/kg,respectively. The method is simple to operate,good accuracy,stability and reproducibility. It can be used for Sudan red analysis in hot pepper products.更多还原