Determination of 5 Fluorescent Whitening Agents in Cosmetics and Detergent by High Performance Liquid Chromatography
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摘 要
采用高效液相色谱法测定化妆品和洗涤剂中荧光增白剂C.I.85,C.I.210,C.I.220,C.I.351和C.I.353。1.000 g化妆品样品或0.500 g洗涤剂样品加入10.0 mL乙腈(1+2)溶液,涡旋振荡1 min后超声提取10 min,以10 000 r·min-1转速离心5 min,上清液经0.22 μm滤膜过滤后,在MG C18色谱柱(250 mm×4.6 mm,5 μm)上分离,以乙腈和含2 mmol·L-1乙酸二正己基铵的10 mmol·L-1乙酸铵溶液为流动相进行梯度洗脱,采用二极管阵列检测器,在波长350 nm处进行检测。5种荧光增白剂的质量浓度均在5.0~100 mg·L-1内与对应的色谱峰面积呈线性关系,检出限(3S/N)在4~20 mg·kg-1之间,测定下限(10S/N)在15~70 mg·kg-1之间。对空白样品在5.0,50,100 mg·L-1等3个浓度水平上进行加标回收试验,回收率在80.3%~111%之间。对样品中的5种荧光增白剂进行6次平行测定,测定值的相对标准偏差在2.4%~8.9%之间。
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Abstract
A method of high performance liquid chromatography was developed to determine 5 fluorescent whitening agents, including C.I. 85, C.I. 210, C.I. 220, C.I. 351 and C.I. 353, in cosmetics and detergent. The sample (1.000 g of cosmetics or 0.500 g of detergent) was mixed well with 10.0 mL of acetonitrile (1+2) solution by vortex oscillation for 1 min, and then ultrasonically extracted for 10 min. After the mixture was centrifugated at 10 000 r·min-1 for 5 min, the supernatant was filtered through a 0.22 μm filter membrane, and seperated on a MG C18 column (250 mm×4.6 mm, 5 μm), with a mixture of acetonitrile and 10 mmol·L-1 ammonium acetate solution (containing 2 mmol·L-1 di-n-hexyl-ammonium acetate) for gradient elution. A diode array detector was used for detection at the wavelength of 350 nm. Linear relationships were found between peak areas and mass concentrations of the 5 fluorescent whitening agents in the same range of 5.0-100 mg·L-1, with detection limits (3S/N) in the range of 4-20 mg·kg-1, and lower limits of determination (10S/N) in the range of 15-70 mg·kg-1. Tests for recovery was made to blank samples at mass contentrations of 5.0, 50, 100 mg·L-1, giving values of recovery between 80.3% and 111%. The 5 fluorescent whitening agents in the samples were determined in parallel for 6 times, and the relative standard deviations of the measured values were between 2.4% and 8.9%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201812007
所属栏目 工作简报
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收稿日期 2018/3/2
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备注顾宇翔,博士研究生,主要从事化妆品和食品检测工作,guyuxiang1@sina.com
引用该论文: GU Yuxiang,YANG Jinqing,WANG Lei. Determination of 5 Fluorescent Whitening Agents in Cosmetics and Detergent by High Performance Liquid Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(12): 1400~1404
顾宇翔,杨晋青,王磊. 高效液相色谱法测定化妆品和洗涤剂中5种荧光增白剂的含量[J]. 理化检验-化学分册, 2018, 54(12): 1400~1404
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参考文献
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【2】戈弋,甘宏宇,陈治淮,等.我国荧光增白剂标准化工作回顾及发展思考[J].上海染料, 2014,42(1):35-42.
【3】GESSNER J, WIRTH M, KIRSCHBAUM F, et al. Caviar composition in wild and cultured sturgeons-impact of food sources on fatty acid composition and contaminant load[J]. Journal of Applied Ichthyology, 2010,18(4/5/6):665-672.
【4】MOL S, TURAN S. Comparison of proximate, fatty acid and amino acid compositions of various types of fish roes[J]. International Journal of Food Properties, 2008,11(3):669-677.
【5】沈永嘉,李红斌,路炜.荧光增白剂[M].北京:化学工业出版社, 2004.
【6】郭惠萍,张美云,刘亚恒.荧光增白剂的毒性分析[J].湖南造纸, 2007(4):43-45.
【7】巨敏,李宏伟,张晨,等.荧光增白剂在洗涤剂中的应用研究[J].精细与专用化学品, 2012,20(2):45-46.
【8】陈海兰,王泽云,李鹏.荧光增白剂对洗衣粉白度与去污及织物增白的影响[J].日用化学工业, 2007,37(2):131-134.
【9】张彪,梁斌,张明玲,等.荧光增白剂在洗衣粉中的效能研究[J].日用化学工业, 2002,32(4):75-78.
【10】刘虎威.实用色谱技术问答[M].北京:化学工业出版社, 2009.
【11】冼燕萍,郭新东,罗海英,等.固相萃取-超高效液相色谱分离测定洗涤用品中4种荧光增白剂[J].色谱, 2013,31(2):162-169.
【12】马会娟,马强,白桦,等.洗涤用品中5种荧光增白剂的高效液相色谱法检测及质谱确证[J].分析试验室, 2014,33(5):569-573.
【13】许健,陶琳,张苗,等.液相色谱-串联质谱法测定发泡聚苯乙烯餐具中8种荧光增白剂的含量[J].理化检验-化学分册, 2017,53(5):512-516.
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