Simultaneous Determination of 10 Dye Components in Hair Dye by High Performance Liquid Chromatography
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摘要: 建立了一种高效液相色谱法同时测定染发剂中对苯二胺等10种氧化型染料组分的检测方法.选用色谱柱Poroshell 120 Bonus-RP,针对对苯二胺、间苯二酚、对氨基苯酚、间氨基苯酚、4-氨基间甲酚、氢醌、4-氨基-2-羟基甲苯、2-硝基对苯二胺、甲苯-2,5-二胺硫酸盐和6-羟基吲哚等10种染料组分进行分析测定.方法在0.01~0.50 mg/mL质量浓度范围内线性相关系数为0.999 86~0.999 96,RSD小于5.91%,回收率为87.2%~106.7%.方法具有简单、快捷、分离效果好等特点.Abstract: In this article a simultaneous analytical method for the detection of P-phenylene diamine and other 10 oxidation type dye components in hair dye by high performance liquid chromatography is described. The objectives of dye derivatives p-phenylenediamine, resorcine, p-aminopheno, m-aminophenol, 4-amino-m-cresol, hydroquinone, 4-amino-2-hydroxytoluene, p-diamino-2-nitrobenzene, 2, 5-diaminotoluene sulfate, 6-hydroxyindole were seperated on a Poroshell 120 Bonus-RP capillary column. Mass spectrometry was used to quantify the dye in hair dye. Results showed that correlation coefficients of the method were from 0.999 85 to 0.999 96. The relative standard deviation(RSD) was less than 5.91% when the concentrations were in the range of 0.01~0.5 mg/mL, the recovery was from 87.2% to 106.7%. The determination results demonstrated that the method had the feature of simple, rapid, and higly selective.
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Key words:
- hair dye /
- dye /
- high performance liquid chromatography
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图 1 染料标准溶液液相色谱图
(1)对苯二胺,(2)间苯二酚,(3)对氨基苯酚,(4)间氨基苯酚,(5) 4-氨基间甲酚,(6)氢醌,(7) 4-氨基-2-羟基甲苯,(8) 2-硝基对苯二胺,(9)甲苯-2, 5-二胺硫酸盐,(10) 6-羟基吲哚
Figure 1. Liquid chromatogram of dye standard soloution
(1) p-phenylenediamine, (2) Resorcine, (3) p-Aminophenol, (4) m-Aminophenol, (5) 4-Amino-m-cresol, (6) Hydroquinone, (7) 4-Amino-2-hydroxytoluene, (8) p-Diamino-2-nitrobenzene, (9) 2, 5-Diaminotoluene sulfate, (10) 6-Hydroxyindole
表 1 洗脱条件
Table 1. Elution conditions
时间/min 流动相A(10 mmol/L乙酸铵)/% B(乙腈)/% 0 95 5 2.0 95 5 8.0 80 20 10.0 10 90 12.5 10 90 13.0 95 5 16.0 95 5 表 2 线性方程、相关系数与检出限
Table 2. Liner equations, correlation coefficients and detection limits
染料组分 线性方程 线性相关系数(R) 检出限/(mg/L) 对苯二胺 Y=4.07X-0.60 0.9999 1 8.0 间苯二酚 Y=2.27X+0.99 0.9999 0 5.0 对氨基苯酚 Y=6.44X=2.41 0.9998 6 8.0 间氨基苯酚 Y=3.98X+1.71 0.9999 0 5.0 4-氨基间甲酚 Y=4.06X+0.04 0.9999 2 8.0 氢醌 Y=4.59X+1.16 0.9999 3 6.0 4-氨基-2-羟基甲苯 Y=2.60X+0.24 0.9999 2 6.0 2-硝基对苯二胺 Y=6.26X+2.29 0.9999 4 10.0 甲苯-2, 5-二胺硫酸盐 Y=4.55X-0.35 0.9999 1 3.0 6-羟基吲哚 Y=3.28X+1.24 0.9999 6 4.0 表 3 染发剂中染料3个添加水平下染料组分加标回收率和相对标准偏差(n=6)
Table 3. Spiked recoveries and RSDs of dye components in hair dye(n=6)
染料组分 加标质量/μg 本底质量/μg 回收质量/μg 回收率/% RSD/% 对苯二胺 625.0 1 705.0 667.5 106.7 2.21 1 250.0 1 252.5 100.2 1.46 2 500.0 2 442.5 97.7 5.05 间苯二酚 625.0 1 453.0 560.0 89.6 3.24 1 250.0 1 180.0 94.3 1.05 2 500.0 2 490.0 99.6 1.13 对氨基苯酚 625.0 / 572.5 91.6 5.91 1 250.0 1 100.0 87.9 2.33 2 500.0 2 340.0 93.6 3.64 间氨基苯酚 625.0 / 642.5 102.8 1.06 1 250.0 1 192.5 95.3 1.16 2 500.0 2 435.0 97.4 2.69 4-氨基间甲酚 625.0 / 612.5 97.9 1.44 1 250.0 1 322.5 105.8 2.09 2 500.0 2 217.5 88.7 1.12 氢醌 625.0 / 577.5 92.5 2.94 1 250.0 1 182.5 94.6 0.87 2 500.0 2 260.0 90.4 1.08 4-氨基-2-羟基甲苯 625.0 / 617.5 98.9 1.41 1 250.0 1 195.0 95.6 3.18 2 500.0 2 407.5 96.3 2.94 2-硝基对苯二胺 625.0 / 545.0 87.2 2.90 1 250.0 1 145.0 91.6 3.81 2 500.0 2 367.5 94.7 1.13 甲苯-2, 5-二胺硫酸盐 625.0 2 925.0 579.5 95.4 1.57 1 250.0 1 120.0 89.6 2.67 2 500.0 2 330.0 93.2 3.12 6-羟基吲哚 625.0 / 590.0 94.5 2.83 1 250.0 1 140.0 91.2 3.71 2 500.0 2 537.5 101.5 2.67 -
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