QB/T 2333-1997 Quantitative determination of ultraviolet absorbers in sunscreen cosmetics by high performance liquid chromatography
Some standard content:
QB/T 2333---1997
Ultraviolet absorbers used in cosmetics can reduce or completely absorb ultraviolet rays and protect the skin. However, if excessive or prohibited ultraviolet absorbers are used, it is easy to irritate the skin and cause skin allergies. The use of ultraviolet absorbers is strictly managed and restricted internationally. GB7916-1987 "Hygiene Standards for Cosmetics" also stipulates the types and limited amounts of ultraviolet absorbers allowed in cosmetics. In order to implement the hygiene standards and keep pace with the international standards, this standard is specially formulated to determine the content of ultraviolet absorbers in sunscreen cosmetics. This standard is formulated based on the principle that different ultraviolet absorbers have different phase distributions on liquid chromatography, are eluted in sequence by the mobile phase, and can be detected by the ultraviolet detector.
Appendix A, Appendix B, and Appendix C of this standard are all standard appendices. This standard can separate fifteen ultraviolet absorbers at a time. The method in Appendix C (standard appendix) can separate five ultraviolet absorbers, and a total of nineteen ultraviolet absorbers can be quantitatively determined. The method is simple and fast. This standard was proposed by the Quality Standards Department of China Light Industry General Association. This standard is under the jurisdiction of the National Cosmetics Standardization Center. The drafting unit of this standard is Beijing Daily Chemical Research Institute. The main drafters of this standard are Xu Wei and Du Xiaohao. 92
1 Scope
Light Industry Standard of the People's Republic of China
Quantitative determination of ultraviolet absorbers in sunscreen cosmetics by high performance liquid chromatography
This standard specifies the high performance liquid chromatography method for determining the content of ultraviolet absorbers in cosmetics. QB/T 2333—1997
This standard is applicable to the separation and quantitative determination of 19 kinds of ultraviolet absorbers in sunscreen cosmetics. The minimum detection amount and detection concentration are shown in Appendix A (Appendix to the standard).
2 Method Summary
The sample is dissolved, extracted and separated with a mixed solvent. After the clear liquid is filtered, the various ultraviolet absorber components are separated by high performance liquid chromatography, and the retention time is used for qualitative determination, and the content is determined by external standard method or working curve method. 3 Reagents and materials
3.1 Preparation of mixed solution
a) Tetrahydrofuran: analytical grade,
b) Methanol: analytical grade;
c) Perchloric acid: high grade (70%),
d) Distilled water: double distilled;
e) Mixed solution: methanol: tetrahydrofuran: water: perchloric acid - 60:100:80:0.05 (volume ratio). 3.2 The preparation of standard stock solutions of various ultraviolet absorbers is shown in Appendix B (Standard Appendix). 3.3 0.5μm fat-soluble sample filter membrane and filter. 4 Instruments and equipment
a) High performance liquid chromatograph, including data processing system and printer or integrator; b) Micro syringe: 25μL,
c) Ultrasonic cleaner.
5 Chromatographic separation conditions
When the sunscreen cosmetic contains two or more of the three UV absorbers Uvinul MS40, ParsolHS, and Uvinul DS49, or contains Uvinul T150 and Uvinul P25, the reference chromatographic separation conditions in Appendix C (Standard Appendix) shall be used for determination. In addition, when the cosmetic contains one or more UV absorbers specified in the scope of application of this standard, this chromatographic separation condition shall be used.
a) Chromatographic column: stainless steel YWG-C18 column, 250mm×4.6mm (or C18 column of the same type); b) Mobile phase: mixed solution (3.le), filtered through a 0.5um filter membrane and degassed; c) Flow rate: 1.0 mL/min;
Approved by China Light Industry Federation on December 4, 1997
TKAONKAca-
Implementation on August 1, 1998
QB/T2333—1997
d) Detector: UV detector, detection wavelength of 310nm; e) Detection sensitivity: 0.05aufs; f) Injection volume: 10 μL.
6 Analysis steps
6.1 Sample pretreatment
Weigh 0.5g of sunscreen cosmetics in a 50mL beaker, accurate to 0.001g, add 25mL of mixed solution (3.1e), fix the beaker in an ultrasonic cleaner and oscillate for 15 to 20 minutes. After the sample is completely dispersed, transfer the solution to a 100mL volumetric flask, wash the beaker with the mixed solution (3.1e for more than three times, add the washing solution to the volumetric flask, and dilute to the scale. When the sample solution is an emulsion, centrifuge part of the solution, take the upper clear liquid and filter it with a sample filter and 0.5 6.2 Preparation of the sample
According to the content of the ultraviolet absorber in the sample (the ultraviolet absorber has a complete chromatogram on the chromatogram), select a dilution factor of 5 to 50 times, dilute the filtrate to be used (6.1) with the mixed solution (3.1e) to prepare the sample to be tested. 2
6.3 Draw the working curve
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1—MS-40 P-HS DS-49 P-25;2—PABA;3-D-50;4—SS-Na+5—M-40;6—Salo1;7--S-22;8—P-5 000;9--P-0;10--E-8020;11--P-1789;12-N-539;13--P-MCX;14-HMS;15-E-587;16-HMS Figure 1 Sequence of peaks of various UV absorbers separated by chromatographic conditions 6.3.1 Preparation of UV absorber series standard solutions When drawing the working curve of each UV absorber, take 0,000 of the standard stock solution of the UV absorber in Appendix B (Standard Appendix) respectively. .10, 0.20, 0.50, 1.00, 2.00mL in a 100ml volumetric flask, dilute to scale with the mixed solution (3.1e), and set aside.
6.3.2 Use a microsyringe to take 10uL of the standard solution in 6.3.1 and inject it into the high performance liquid chromatograph, and record the retention time and peak area of the chromatogram. Plot the peak area against the concentration of the standard ultraviolet absorber (g/mL) to obtain the working curve. 6.4 Determination of the anti-corrosion sample to be tested
Use a microsyringe to take 10 μL of the sample to be tested (6.2) and inject it into the HPLC, and record the retention time and peak area of each chromatographic peak.
7 Calculation
QB/T2333-1997
7.1 External standard method to calculate the percentage of the tested ultraviolet absorber X,=c;X
Where: X;——Percentage of the tested ultraviolet absorber, %, c
Concentration of standard ultraviolet absorber test solution, name/mL; Standard ultraviolet absorber Peak area of the tested ultraviolet absorber;
The peak area of the tested ultraviolet absorber;
The volume of the tested sample solution diluted, mL; The weight of the tested sample, g.
7.2 Working curve method to calculate the percentage of the tested ultraviolet absorber X, =
Where: X,
The percentage of the tested ultraviolet absorber, %, The volume of the tested sample solution diluted, mL
The concentration of the ultraviolet absorber found on the curve, g/mL; The weight of the tested sample, g.
The arithmetic mean of the results of two parallel measurements is the content of the tested ultraviolet absorber. 7.3 Precision
The relative deviation of two parallel determination results is less than 5%. TKAONKAca-
（2）
A1 See Table A1.
QB/T 2333--1997
Appendix A
(Appendix to the subject matter)
Name, CAS number, usage limit and minimum detection amount of ultraviolet absorbers determined by this methodTable A1Name, CAS number, usage limit and minimum detection amount of ultraviolet absorbers determined by this methodChinese name
English name
Aminobenzoic acid
Aminobenzoic acid
Para-nitrobenzoic acid
Ethoxylated ethyl-4-
Acid oxyethylene
Aminobenzoate
2-Ethylhexyl-4-dimethyl-
Dimethylamino
Octyl benzoate
Aminobenzoate
Homosalate
Octyl salicylate 2-Ethylhexyl Sodium salicylate
Sodium salicylate
Phenyl salicylate
Methoxycinnamate
2-Ethylhexyl-4-
Octyl esterwwW.bzxz.Net
Methoxycinnamate
Oxybenzophenone-3|Oxybcnzone
2.2',4.4°-2'2,4,4'-Tetrahydroxy-Tetrahydroxy-diphenyl
benzophenone
Benzophenone-
5-sulfonic acid
2-Hydroxy-4-methoxybe-
nzophenone 5-sulfonic acid
[2.2'-Dihydroxy 2,2′-Dihydroxy-4.4′-yl-4, 4'-- dimethoxy benzophenone 5.5'-disulfonate
Methoxybenzene-5.5
Registration number
150-13-0
113010-
Trade name or common name
(Manufacturer)
PABA(domestic)
PEG-25 PABA.
Uvinul P-25(BAFS)
21245-02-3Octyl dimethyl PABA,PadimateQ, Escalol 507 (ISP Van Dyk),Eusolex 6007(Rona/E.Merck)
118-56-9 Eusolex HMS(Rona/E. Merck)Escalol 587(ISP Van Dyk)
118-60-5
532-32-1
93-99-2
The code used in this article is SS-Na (domestic)
Salol (domestic)
Escalol 557 (ISP Van Dyk).
5466-77-3
Eusolex 2292(Rona/E. Merck).Uvinul MC 80(BASF).
Parsol MCX(Hoffmann-LaRoche)131-57-7
131-55-5
Benzophenone-3.
Escalol 567(ISP Van Dyk),
Eusolex 4360(Rona/E.merck),
Uvinul M-40(BASF)
Benzophenone-2.
Uvinul D-50(BASF)
Benzophenone-4,
4065-45-6
Uvinul MS-40(BASF)
Benzophenone-9,
Uvinul DS-49(BASF)
This standard
Use commodity
Abbreviation
Minimum detection
Detection concentration
SS-Na|2(acid)
Chinese name
Isopropyl dibenzoylmethane
Formyl methane
Camphor
3,4°-methyl
Camphor
English name
Isopropyl
dibenzoylmethane
3-Benzylidene camphor
4-Methyl benzylidene
camphor
tert-butyl-methylButyl methoxydibenzoyl-dibenzoyl methane
oxygen
octyl triazone triazone
2-cyano-3,
2-Ethylhexyl 2-cyano-3.
3'-diphenyl-carylate
2-Phenyl benzimidazole
5-sulfonic acid and salts
QB/T 2333--1997
Table A1 (end)
Registration No.
Trade Name or Common Name
(Manufacturer)
Eusolex 8020(Rona/E. Merck)
63250-25-91
15087-24-8Mexoryl SD(Chimex)38102-62-41
Eusolex 6300(Rona/E. Merck).Parsol 5000(Hoffmann-LaRoche)Eusolex 9020(Rona/E. Merck).70356-09-111
Parsol 1789(Hoffmann-LaRoche)88122-99-0 Uvinul T-150(BASF)6197-30-4
Uvinul N539 SG(BASF).
Escalol 597(ISP Van Dyk),
Eusolex OCR(Rona/E. Merck)
27503-81-7Eusolex232(Rona/E.Merck)Parsol HS(Hoffmann-LaRoche)
Appendix B
(Standard Appendix)
Preparation of UV absorber standard stock solution This standard
Uses the product
Abbreviation
E-8020
P-5000
P-1789
Minimum!
Minimum detection
Pick out the measured concentration
P-HS8 (acid)
4 (salt)
Weigh the UV absorber standard sample into a 100mL volumetric flask and mix with the mixed solution (3.1e) Dilute to scale. Store at 0-4℃. See Table B1 for the sample weight and concentration of each UV absorber standard sample. Preparation of mixed standard solution of ultraviolet absorbers B2
Table B1 Sample weight and solution concentration of each ultraviolet absorber standard sample solution Ultraviolet absorber trade name (generic name) PABA
Uvinul P-25
Padimate
Eusolex HMS
Escalol 587
Parsol MCx
Ultraviolet absorber standard sample weight
TTiKAoNi KAca-
Concentration of ultraviolet absorber standard solution
Ultraviolet absorber trade name (generic name) Uvinul M-40
Uvinul MS-40
Uvinul D-50
Uvinul DS-49
Eusolex 8020
Mexoryl SD,(Unisol S-22)
Parsol5000
Parsol 1789
Uvinul T150
Uvinul N539
Parsol HS
QB/T 2333—1997
Table BI (end)
Weighing amount of standard UV absorbers
Appendix C
(Appendix of standard)
Reference separation conditions of liquid chromatography
Concentration of UV absorber standard solution
C1Reference chromatographic condition 1: Applicable to the separation and quantitative determination of each UV absorber when two or more of the three UV absorbers of Uvinul MS-40, Parsol HS and Uvinul DS-49 exist at the same time. See Figure C1. a) Chromatographic column: same as 5a;
b) Mobile phase: acetonitrile: water m7:93, filtered through 0.5μm filter membrane and degassed; c) Flow rate: 1.4mL/min;
d) Detector: same as 5d;
e) Detection sensitivity: same as 5es
f) Injection volume: same as 5f.
t×10min
Figure C1 Reference chromatographic conditions
Separation of the peak order of three ultraviolet absorbers QB/T 2333—1997
Reference chromatographic conditions 2: Applicable to the separation of two ultraviolet absorbers, UvinulP25 and Uvinul T150, and the quantitative determination of each ultraviolet absorber C2
See Figure C2.
a) Chromatographic column: same as 5a;
b) Mobile phase: methanol: tetrahydrofuran: water: perfluoric acid = 30:90:30:0.05, filtered through a 0.5μm filter membrane and degassed; c) Flow rate: same as 5c;
d) Detector: same as 5d,
e) Detection sensitivity: same as 5e;
f) Injection volume: same as 5f.
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Figure C2 Reference chromatographic conditions 2
Separation of peak sequence of two ultraviolet absorbers TTi KAoNni KAca-
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