高效液相色谱法测定染发剂中2-硝基-p-苯二胺
HPLC Determination of 2-Nitro-p-benzenediamine in Hair Dyes
摘 要
应用高效液相色谱法测定了染发剂中2-硝基-p-苯二胺的含量。样品用乙醇-水(1+1)混合溶液提取后,经水系C18色谱柱分离,以(A) 10 mol·L-1柠檬酸缓冲溶液-10 mol·L-1辛烷磺酸钠溶液(pH 2.6)与(B)乙腈以体积比75比25组成的混合溶液为流动相进行等度洗脱,用二极管阵列检测器于410 nm检测。2-硝基-p-苯二胺的线性范围为2.4~240 mg·L-1,检出限(3S/N)为0.7 mg·L-1。以染发剂样品为基体,进行加标回收试验,回收率在90.4%~99.4%之间,相对标准偏差(n=6)在0.35%~3.0%之间。
2-硝基-p-苯二胺
染发剂
HPLC
2-Nitro-p-benzenediamine
Hair dyes
Abstract
HPLC was applied to the determination of 2-nitro-p-benzenediamine in hair dyes. The sample was extracted with mixture of CH3CH2OH-H2O (1+1). The extract was separated on auqo-C18 column by gradient elution with eluants containing A (10 mol·L-1 citric acid +10 mol·L-1 sodium octanesulfonate of pH 2.6) and B (acetonitrile) mixed in the ratio of 75 to 25, and determined with diode array detector at the wavelengths of 410 nm. Linearity range for 2-nitro-p-benzenediamine was found between 2.4-240 mg·L-1, with detection limit (3S/N) of 0.7 mg·L-1. Using sample of hair dyes as matrix, recovery test was made by standard addition method, values of recovery found were in the range of 90.4%-99.4%, with RSD′s (n=6) in the range of 0.35%-3.0%.
中图分类号 O652.63
所属栏目
基金项目 厦门出入境检验检疫局科技基金(2007XK03)
收稿日期 2011/1/12
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备注赖莺(1978-),女,福建长汀人,高级工程师,博士,主要从事色谱、质谱和光谱等方面的进出口商品检验和科研工作。
引用该论文: LAI Ying,CHEN He-xiu,LIN Rui,WANG Hong-hui,DONG Qing-mu,HUANG Zong-ping. HPLC Determination of 2-Nitro-p-benzenediamine in Hair Dyes[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(2): 185～187
赖莺,陈和秀,林睿,王鸿辉,董清木,黄宗平. 高效液相色谱法测定染发剂中2-硝基-p-苯二胺[J]. 理化检验－化学分册, 2012, 48(2): 185～187
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参考文献
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【14】朱英,杨艳伟,李静.气相色谱-质谱法同时测定氧化型染发剂中的多种染料中间体［J］.色谱, 2005,23(5):566-566．
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【2】KOH D, TAN C, NG S K, et al. Screening for p-phenylenediamine (PPD) in hair-care products by thin-layer chromatography (TLC)［J］. Contact Dermatitis, 2000,43:182-183．
【3】RATOGI S C. A method for the analysis of intermediates of oxidative hair dyes in cosmetic products［J］. J Sep Sci, 2001,24:173-178．
【4】PEL E, BORDIN G, RODRIGUEZ A R. HPLC candidate reference method for oxidative hair dye analysis. I. separation and stability testing［J］. J Liq Chrom & Rel Technol, 1998,21(6):883-901．
【5】VINCENT U, BORDIN G, RODRIGUEZ A R. Validation of an analytical procedure for the determination of oxidative hair dyes in cosmetic formulations［J］. J Cosmetic Sci, 2002,53:43-58．
【6】VINCENT U, BORDIN G, RODNGUEZ A R. Optimization and validation of an analytical procedure for the of oxidative hair dyes in commercial cosmetic formulations［J］. J Cosmetic Sci, 2002,53:101-109．
【7】朱会卷,杨艳伟,张卫强,等.高效液相色谱法测定染发剂中的22种染料成分［J］.色谱, 2008,26(5):554-558．
【8】EGGENREICH K, GOLOUCH S, TOSCHER B, et al. Determination of 4-amino-m-cresol and 5-amino-o-cresol and metabolites in human keratinocytes (HaCaT) by high-performance liquid chromatography with DAD and MS detection［J］. J Biochem Biophys Methods, 2004,61:23-34．
【9】TOKUDA H, KIMURA Y, TAKANO S. Determination of dye intermediates in oxidative hair dyes by fused-silica capillary gas chromatography［J］. J Chromatogr A, 1986,367:345-356．
【10】郑曙昭,李荣专.毛细管气相色谱法测定染发剂中七种染料组分［J］.分析测试技术与仪器, 2003,9(1):26-29．
【11】吴卫平,周世伟,计培鑫.三氟乙酸酐衍生化毛细管气相色谱法测定染发剂中苯二胺含量［J］.中国卫生检验杂志, 1999,9(3):186-188．
【12】DI GIOIA M L, LEGGIO A, LE PERA A, et al. Determination by gas chromatography/mass spectrometry of p-phenylenediamine in hair dyes after conversion to an imine derivative［J］. J Chromatogr A, 2005,1066:143-148．
【13】刘丽,李英,刘志红,等.超声波抽提气相色谱质谱法测定氧化型染发剂中16种染料［J］.分析化学, 2004,32(10):1333-1336．
【14】朱英,杨艳伟,李静.气相色谱-质谱法同时测定氧化型染发剂中的多种染料中间体［J］.色谱, 2005,23(5):566-566．
【15】WANG S P, HUANG T H. Separation and determination of aminophenols and phenylenediamines by liquid chromatography and micellar electrokinetic capillary chromatography［J］. Anal Chim Acta, 2005,534:207-214．
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