Lab Glassware Division 中文(Chinese)

Analysis of 32 Banned and Restricted Chemicals in Hair Dyes

Method: HPLC
Matrix: 0
Application No.: 101947
Componds: Hydroquinone, Resorcinol, 2-Methylresorcinol, 4-Amino-3-nitrophenol, p-Aminophenol,
N,N-bis(2-hydroxyethyl)-p- phenylenediamine sulfate, 6-Hydroxyindole, 4-Chlororesorcinol,
4-Amino-m-cresol, 4-Nitro-o-phenylenediamine, 2,4-Diaminophenoxyethanol HCl,
Phenylmethyl pyrazolone,
2-Nitro-p-phenylenediamine, 2-Chloro-p-phenylenediamine sulfate, 2,7-Naphthalenediol,
N,N-Diethyl-p-phenylenediamine sulfate, 6-Amino-m-cresol, 4-Amino-2-hydroxytoluene,
Toluene-3,4-diamine, N-Phenyl-p-phenylenediamine, 1-Naphthol, 2-Amino-3-hydroxypyridine,
p-Methylaminophenol sulfate, m-Aminophenol, p-Phenylenediamine, m-Phenylenediamine,
o-Aminophenol, Toluene-2,5-diamine sulfate, 2,6-Diaminophenoxyethanol HCl,
o-Phenylenediamine, 1,5-Naphthalenediol, N,N-Diethyltoluene-2,5-diamine HCl

Sample Pretreatment: Standards: Most of the 32 analytes were prepared at a concentration of 5mg/mL using a mixed
solution of methanol and 2g/L sodium bisulfite (1:1 v/v). Some analytes could not be dissolved
thoroughly in the solution mentioned above; therefore, their stock standard solution was prepared
using other suitable solvents. Toluene-2,5-diamine and 2-chloro-p-phenylenediamine sulfate
stock standard solution, both having a concentration of 5mg/mL, were prepared by 2g/L sodium bisulfite.
The same concentration of toluene-3,4-diamine and 4-nitro-o-phenylenediamine solution was prepared
by methanol. 2-Nitro-p-phenylenediamine was dissolved by ethanol to make the final concentration of 2.5mg/mL.
Conditions: Mobile Phase Ⅰ:
A: 40mMPotassium phosphate monobasicbuffer (pH2.8) with 10mMsodium 1-octanesulfonate
B: Acetonitrile/methanol=40:60
Gradient: 10%B hold 10min, 10 to 20%B in 10min, 20 to 30%B in 10min, 30 to 40%B in 10min,
hold 4min, 40 to 60%B in 3min, hold 7min, 60 to 10%B in 0.5min,equilibrate at 10%B for 5.5min

Mobile Phase Ⅱ:
A: 40mMPotassium phosphate monobasic buffer (pH2.8) with 10mM sodium 1-octanesulfonate
B: Acetonitrile
Gradient: 10%B hold 13min, 10 to 20%B in 10min, 20 to 30%B in 10min, 30 to 10%B in 1min,
equilibrate at 10%B for 6 min

Flow Rate: 1.0 mL/min;
Injection: 5µL;
Temperature: 35 0C;
Wavelength: 280nm
Publisher: Dikma Technologies Inc.
Keyword: Hydroquinone, Resorcinol, 2-Methylresorcinol, 4-Amino-3-nitrophenol, p-Aminophenol, N,N-bis(2-hydroxyethyl)-p- phenylenediamine sulfate, 6-Hydroxyindole, 4-Chlororesorcinol, 4-Amino-m-cresol, 4-Nitro-o-phenylenediamine, 2,4-Diaminophenoxyethanol HCl,
Abstract: 32 banned and restricted chemicals can be separated by a reversedphase gradient elution procedure with easy control and high reproducibility.

Chromatogram of 21chemicals mixed solution (mobile phase I)

No.
Compounds
Concentration (mg/mL)
Retention Time(min)
Resolution
Asymmetry
1
Hydroquinone
0.1
6.2
-
1.14
2
Resorcinol
0.17
10.9
20.76
1.15
3
2-Methylresorcinol
0.7
13.1
7.18
1.33
4
4-Amino-3-nitrophenol
0.1
20.5
22.37
0.98
5
p-Aminophenol
1
24.9
10.76
0.86
6
N,N-bis(2-hydroxyethyl)-p- phenylenediamine sulfate
0.17
27.3
6.31
1.04
7
6-Hydroxyindole
0.1
28.9
4.91
1.04
8
4-Chlororesorcinol
0.17
29.8
2.63
1.11
9
4-Amino-m-cresol
0.17
30.4
1.71
1.04
4-Nitro-o-phenylenediamine
0.17
31.0
2.25
1.00
11
2,4-Diaminophenoxyethanol HCl
0.1
31.6
2.43
1.09
12
Phenylmethyl pyrazolone
0.17
32.3
1.25
1.45
13
2-Nitro-p-phenylenediamine
0.17
33.5
1.89
0.97
14
0.08
33.8
1.29
1.00
15
2,7-Naphthalenediol
0.17
35.6
6.06
1.08
16
N,N-Diethyl-p-phenylenediamine sulfate
0.7
37.0
4.96
1.06
17
6-Amino-m-cresol
0.17
39.7
11.58
1.03
18
4-Amino-2-hydroxytoluene
0.17
40.5
3.28
0.99
19
0.17
41.1
2.49
1.01
20
N-Phenyl-p-phenylenediamine
0.015
50.6
48.27
1.16
21
1-Naphthol
0.17
51.9
7.79
1.02

 

Chromatogram of 11 chemicals mixed solution (mobile phase II)

No.
Compounds
Concentration (mg/mL)
Retention Time(min)
Resolution
Asymmetry
1
2-Amino-3-hydroxypyridine
0.08
23.0
-
1.35
2
p-Methylaminophenol sulfate
0.4
24.1
2.68
0.98
3
m-Aminophenol
0.2
25.3
3.94
0.95
4
p-Phenylenediamine
0.2
26.1
2.63
0.91
5
m-Phenylenediamine
0.2
26.5
1.97
0.95
6
o-Aminophenol
0.2
27.3
3.78
0.97
7
Toluene-2,5-diamine sulfate
0.4
27.6
1.66
0.98
8
2,6-Diaminophenoxyethanol HCl
1.11
28.3
3.34
0.85
9
o-Phenylenediamine
0.2
28.9
3.20
0.97
10
1,5-Naphthalenediol
0.2
29.6
2.87
1.06
11
N,N-Diethyltoluene-2,5-diamine HCl
0.2
32.7
12.60
1.10