高效液相色谱法同时测定牙膏及漱口水中的23种致癌染料

建立了同时测定牙膏和漱口水中23种致癌染料的高效液相色谱(HPLC)检测方法。漱口水样品直接以乙醇溶解稀释,牙膏样品烘干后以乙醇超声提取。采用ZORBAX Eclipse XDB-Phenyl(150 mm×4.6 mm×5μm)色谱柱进行分离,以2.5 mmol/L磷酸二氢四丁基铵水溶液(pH 7.5)和甲醇-乙腈(体积比50∶50)为流动相进行梯度洗脱,二极管阵列检测器(DAD)在400、500、600 nm波长下检测,外标法定量。结果表明,23种致癌染料在32 min内完成色谱分离,在相应的质量浓度范围内线性良好,相关系数(r2)均不小于0.9991,检出限(LOD)和定量下限(LOQ)分别为0.06~0.66 mg/L和0.18~1.98 mg/L。以阴性牙膏和漱口水为样品基质,23种致癌染料在3个加标水平下的平均回收率分别为91.2%~104%和92.0%~103%,相对标准偏差(RSD,n=6)分别为2.5%~5.8%和2.3%~5.5%。对239个牙膏和88个漱口水样品进行检测,1个牙膏样品中检出碱性紫3。该方法灵敏度高,精密度好,准确度高,适用于牙膏和漱口水中致癌染料的测定,可为牙膏和漱口水的质量安全监控提供参考。

Simultaneous Determination of 23 Carcinogenic Dyes in Toothpaste and Mouthwash by High Performance Liquid Chromatography

A high performance liquid chromatographic(HPLC)method with innovative sample pretreatment was developed for the simultaneous determination of 23 carcinogenic dyes in toothpaste and mouthwash.The mouthwash sample was directly dissolved and diluted by ethanol.After mixed by vortex with quartz sand,the toothpaste sample was vacuum-dried at 75℃,then ultrasonically extracted with ethanol at 50℃for 30 min.The separation of 23 target analytes was performed on a ZORBAX Eclipse XDB-Phenyl column(150 mm×4.6 mm×5μm)by gradient elution with 2.5 mmol/L tetrabutylammonium phosphate(pH 7.5)and methanol-acetonitrile(50∶50,by volume)as mobile phases.The detection wavelengths for diode array detector(DAD)were 400 nm,500 nm and 600 nm,respectively.Quantitative analysis was carried out by external standard method.Results showed that the chromatographic separation for 23 carcinogenic compounds was achieved within 32 minutes.There were good linear relationships for 23 target analytes in the corresponding concentration ranges with correlation coefficients(r2)not less than 0.9991.The detection limits(LOD)and quantitation limits(LOQ)were in the ranges of 0.06-0.66 mg/L and 0.18-1.98 mg/L,respectively.The average recoveries for 23 carcinogenic dyes in negative toothpaste and mouthwash at three spiked levels were in the ranges of 91.2%-104%and 92.0%-103%,with their relative standard deviations(RSD,n=6)of 2.5%-5.8%and 2.3%-5.5%,respectively.239 toothpaste and 88 mouthwash samples were detected by this method,and basic violet 3 was detected in a toothpaste sample.With the advantages of high sensitivity,good precision and satisfactory accuracy,the method is suitable for the quantitative analysis of 23 carcinogenic dyes in all kinds of toothpaste and mouthwash,and provides a good strategy reference for the quality and safety monitoring of toothpaste and mouthwash.