建立了测定胶囊壳中20种禁用工业染料的高效液相色谱-二极管阵列检测器法。样品经乙腈-甲醇溶液(1:2, V/V)超声提取3次,以Agilent ZORBAX Eclipse Plus C18柱为分析柱,用乙腈和含0.3%三乙胺,0.2% H3PO4溶液(pH 2.7)进行梯度洗脱,同时在360、420、460、570和630 nm的检测波长下监测。结果表明,20种禁用工业染料在0.5~20μg/mL浓度范围内线性关系良好,相关系数为0.9991~1.0000,检出限为0.05~0.27μg/mL。在1,3和10μg/g加标水平下,20种禁用工业染料的回收率为64.1%~114.9%,日内及日间的相对标准偏差分别为0.4%~9.9%和0.9%~9.9%,定量限为0.16-2.33μg/g。本方法操作简单,分析快速,灵敏度好,适用于胶囊壳中禁用工业染料的日常检测。
A high performance liquid chromatography with diode array detection method (HPLC-DAD) was established for determination of 20 forbidden industrial dyes in capsule shells. The capsule shell samples were repeatedly extracted three times under ultrasonication with acetonitrile-methanol solution (1:2, V/V). The extract was separated on Agilent ZORBAX Eclipse Plus C18 column with gradient elution by using acetonitrile and 0.3% triethylamine, 0.2% phosphoric acid aqueous solution (pH 2.7) as eluant, and then monitored under the detection wavelength of 360, 420, 460, 570 and 630 nm. The results showed that the linearity of 20 forbidden industrial dyes ranged from 0.5 to 20 μg/ml with correlation coefficients of 0.9991-1.0000. The limit of detection of the instrument was 0.05 to 0.27 μg/mL. The recoveries of these dyes (spiked at levels of 1, 3, and 10 μg/g) ranged from 64.12% to 114.89%, while intra-day and inter-day relative standard deviations ranged from 0.4% to 9.9% and 0.9% to 9.9%, respectively. The Limit of quantification of the method was 0.16-2.33 μg/g. This method is sample, rapid and sensitive, and suitable for routine determination of the forbidden industrial dyes in capsule shells.
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