Simultaneous Determination of 19 Synthetic Colorants in Toothpaste by High Performance Liquid Chromatography
  
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KeyWord:synthetic colorant  toothpaste  simultaneous determination  high performance liquid chromatography(HPLC)
  
AuthorInstitution
SHI Xing-hong,LUO Jin-mei,YANG Dan-mei,FU Qiu-mei,QIU Ying-heng,WU Xiao-ou,WANG Xiao-wei Shenzhen Institue for Drug Control,NMPA Key Laboratory for Monitoring and Evaluation of Cosmetics,Shenzhen ,China
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Abstract:
      The colorants in toothpastes are mainly synthetic colorants,which may cause varying degrees of harm to the human body with long-term or excessive use.However,there is a lack of research on effective methods for detection of colorants in toothpastes.In this study,a high performance liquid chromatographic(HPLC) method was established for the simultaneous determination of 19 synthetic colorants in toothpastes.The samples were dispersed using 4 mL water with a vortex mixer,then defoamed with 1.0 mL of methanol,and finally added water to 9 mL.The ultrasonic extraction was performed for 10 min.The solution was added water to volume of 10 mL,centrifuged at 10 000 r/min for 5 min,and filtered through 0.45 μm hydrophobic microporous poly tetra fluoroethylene(PTFE).Chromatographic separation was achieved on an Agilent eclipse XDB-C18 column(4.6 mm × 150 mm,5 μm) by gradient elution,using acetonitrile-20 mmol/L ammonium acetate(pH 6.0) as mobile phase at a flow rate of 0.7 mL/min and a column temperature of 35 ℃.The multi-wavelength analysis was carried out by means of a diode array detector,and the external standard method was used for quantification.The results showed that the 19 synthetic colorants had good linearities in the range of 1-50 mg/L,with correlation coefficients(r) greater than 0.999.The detection limits of the method were in the range of 0.3-2.6 μg/g and the quantitation limits were 0.9-8.6 μg/g.At two spiked levels of 25 μg/g and 400 μg/g,the average recoveries for the 19 colorants were in the range of 95.2%-103%,with relative standard deviations(RSD,n = 6) less than 5%.This method was used for the determination of 19 colorants in 25 batches of toothpastes on the market.As a result,Food Blue 2 was detected in 7 batches of samples with content of 1.1 - 17.8 μg/g. Food Yellow 4 was detected in 4 batches of samples with content of 4.8 - 31.1 μg/g.Food Yellow 3 was detected in 4 batches with content of 2.6-25.5 μg/g.Food Yellow 4,Food Blue 2 and Food Yellow 3 were detected simultaneously in one batch of samples.Food Red 12,Food Green 3 and Acid Red 92 were detected in three batchs of samples,respectively,with contents of 4.5、1.1、55.3 μg/g,respectively,The other colorants were not detected.The results indicated that the method was simple,rapid,accurate and reliable,and was suitable for the qualitative and quantitative detection of 19 synthetic colorants in toothpastes.
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