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建立了高效液相色谱法同时测定化妆品中颜料红4等38种限用着色剂的检测方法。样品经四氢呋喃、甲醇、乙酸铵水溶液混合溶剂超声提取后,经离心、氮吹和复溶,于 Agilent zorbax SB-Aq 色谱柱(150 mm×3.0 mm,3.5μm)上进行反相液相色谱分离,以乙腈和含0.075%( v/v)甲酸的30 mmol/L乙酸铵溶液为流动相进行梯度洗脱。选择254、416、484、514、590和620 nm作为检测波长进行定量分析。结果表明:在1~10 mg/L 的质量浓度范围内,38种限用着色剂的色谱峰面积与质量浓度呈线性相关,相关系数( r)大于0.999,LOQ 值为5~50μg/g。在100μg/g和500μg/g两个加标水平下,各目标化合物回收率均在93.2%~107.6%之间,相对标准偏差( RSD)小于10%( n=6)。该方法简便、快速、灵敏度高、重现性好,适合于化妆品中限用着色剂的定性与定量检测。

A method has been established for the simultaneous determination of 38 limited col-orants in cosmetics by high performance liquid chromatography( HPLC ). The samples were extracted by ultrasonic with tetrahydrofuran,methanol,ammonium acetate solution as extrac-tion solvents. After centrifugation,nitrogen blow and redissolved in turn,the extracts were separated on an Agilent zorbax SB-Aq column(150 mm×3. 0 mm,3. 5 μm)using a gradient elution program with acetonitrile and 30 mmol/L ammonium acetate containing 0. 075%( v/v) formic acid as mobile phases. The detection wavelengths were set at 254,416,484,514,590 and 620 nm. The linear ranges of the 38 target compounds were all in the range of 1 to 10 mg/L with correlation coefficients more than 0. 999. The limits of quantification( LOQs)for the 38 colorants were in the range of 5—50 μg/g. The average recoveries at two spiked levels ranged from 93. 2% to 107. 6% with the relative standard deviations( RSDs ) less than 10%( n=6 ). This method is accurate,simple,sensitive and reliable,and can be used for the analysis of the 38 limited colorants in cosmetics.

参考文献

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