深圳市药品检验研究院,国家药品监督管理局化妆品监测评价重点实验室,广东 深圳 518000
邱颖姮,硕士研究生,主任药师,研究方向:化妆品质量标准研究与风险监测评价,E-mail:1162593792@qq.com
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石兴红,罗金梅,杨淡梅等.高效液相色谱法同时检测牙膏中19种合成着色剂[J].分析测试学报,2022,41(03):392-397.
SHI Xing-hong,LUO Jin-mei,YANG Dan-mei,et al.Simultaneous Determination of 19 Synthetic Colorants in Toothpaste by High Performance Liquid Chromatography[J].Journal of Instrumental Analysis,2022,41(03):392-397.
石兴红,罗金梅,杨淡梅等.高效液相色谱法同时检测牙膏中19种合成着色剂[J].分析测试学报,2022,41(03):392-397. DOI: 10.19969/j.fxcsxb.21071502.
SHI Xing-hong,LUO Jin-mei,YANG Dan-mei,et al.Simultaneous Determination of 19 Synthetic Colorants in Toothpaste by High Performance Liquid Chromatography[J].Journal of Instrumental Analysis,2022,41(03):392-397. DOI: 10.19969/j.fxcsxb.21071502.
建立了高效液相色谱法(HPLC)同时测定牙膏中19种合成着色剂的检测方法。样品经水分散后超声提取,以10 000 r/min离心5min,经0.45 μm微孔聚四氟乙烯(PTFE)过滤后取滤液测定。采用Agilent eclipse XDB-C,18,柱(4.6 mm × 150 mm,5 μm),以乙腈和20 mmol/L乙酸铵溶液(pH 6.0)为流动相进行梯度洗脱,流速0.7 mL/min,柱温35 ℃,二极管阵列检测器多波长检测,外标法定量。结果表明,19种合成着色剂在1~50 mg/L范围内线性关系良好,相关系数(,r,)均大于0.999;方法检出限为0.3~2.6 μg/g,定量下限为0.9 ~ 8.6 μg/g。在25 μg/g和400 μg/g两个加标水平下,19种着色剂的平均回收率为95.2%~103%,相对标准偏差(RSD,,n ,= 6)小于5%。该方法操作简便、快速、准确,适合于牙膏中多种合成着色剂的定性与定量检测。
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-C,18, 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.
合成着色剂牙膏同时检测高效液相色谱法(HPLC)
synthetic coloranttoothpastesimultaneous determinationhigh performance liquid chromatography(HPLC)
GB/T 8372-2017.Toothpaste. National Standards of the People’s Republic of China(牙膏.中华人民共和国国家标准).
Tang J,Fei X Q,Fu W,Zhou J,Ding Y C,Qian K,Dong S W,Cao L H.J. Instrum. Anal. 汤娟,费晓庆,富薇,周佳,丁友超,钱凯,董绍伟,曹丽华.分析测试学报),2021,40(3):356-362.
Zhu H Y,Huang W Q.J. Mod. Med. Health(朱海英,黄万琪.现代医药卫生),2011,27(8):1259-1261.
Wang H W,Liu S L,Zhao M,Cao J,Huang B N,Niu Z R.J. Food Saf. Qual. (王宏伟,刘素丽,赵梅,曹进,黄丙楠,钮正睿.食品安全质量检测学报),2019,10(1):1-7.
National Medical Products Administration. Safety and Technical Standards for Cosmetics(国家食品药品监督管理总局.化妆品安全技术规范),2015.
Council State. Cosmetics Regulatory Rules(国务院.化妆品监督管理条例).[2021-06-24].https: //www.nmpa.gov.cn/xxgk/fgwj/flxzhfg/20200629190501801.htmlhttps://www.nmpa.gov.cn/xxgk/fgwj/flxzhfg/20200629190501801.html.
Fu Y,Zhu Y,Wu Y L.J. Instrum. Anal. (付岩,朱勇,吴银良.分析测试学报),2017,36(4):496-501.
Li X L,Zhang F M,Fan D Q,Cai H C,Gao L,Wang Q H,Hu Y,Li C.China Meas. Test(李响丽,张凤梅,范多青,蔡昊城,高莉,王庆华,胡燕,李超.中国测试),2021,47(3):76-81.
Pan C,Wu L,Xie Y,Xu W Q,Bai Y,Huang Y H,Hu Z Y.Chin. J. Chromatogr.
潘城,吴凌,谢勇,许文琪,白洋,黄永辉,胡朝阳.色谱),2018,36(9):904-910.
Xie N.J. Food Safe. Qual.(谢楠.食品安全质量检测学报),2021,12(4):1524-1530.
Hu J T,Liu X R,He C Y,Yu L Y,Chen Y F,Li D D,Yu G.J. Food Saf. Qual. 胡江涛,刘兴睿,何成艳,俞凌云,陈艺锋,李丹丹,于刚.食品安全质量检测学报),2019,10(19):6456-6461.
Yang D M,Qiu Y H,Wu X O,Xiong X T,Xia Z M,Li Q.J. Shenyang Pharm. Univ. (杨淡梅,邱颖姮,邬晓鸥,熊小婷,夏泽敏,李清.沈阳药科大学学报),2020,37(9):778-808.
Wu T P,Zhang J C,Ma K.J. Instrum. Anal. (武太鹏,张京晨,马康.分析测试学报),2019,38(2):207-212.
Ju L Y,Li Z J,Song W D,Xu C G,Cui J.J. Instrum. Anal. (鞠玲燕,李兆杰,宋卫得,徐成钢,崔嘉.分析测试学报),2019,38(8):931-938.
Li W,Ai L F,Ma Y S,Chen R C,Guo C H.J. Anal. Sci. (李玮,艾连峰,马育松,陈瑞春,郭春海.分析科学学报),2020,36(1):75-80.
Zhang S,Hu Q,Sun J,Feng R,Yu H,Ji S.World Chin. Med. (张甦,胡青,孙健,冯睿,于泓,季申.世界中医药),2019,14(4):822-832.
Nie L,Ge S L,Yang J Q,Qin Y,Yu C H,Lu Z Y.Flavour Fragrance Cosmetics(聂磊,葛淑丽,杨晋青,秦宇,虞成华,陆志芸.香料香精化妆品),2019,(2):27-32.
Jiang Z B,Ren G J,Mao X Q,Li C L,Zhang G C,Wang L Z.J. Instrum. Anal. (姜子波,任国杰,毛希琴,李春玲,张国翠,王灵芝.分析测试学报),2016,35(7):792-798.
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