GB/T 35829-2018 PDF in English
GB/T 35829-2018 (GB/T35829-2018, GBT 35829-2018, GBT35829-2018)
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Determination of four naphthalenediols in cosmetics -- High performance liquid chromatography
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Standards related to: GB/T 35829-2018
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GB/T 35829-2018: PDF in English (GBT 35829-2018) GB/T 35829-2018
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.70
Y 42
Determination of Four Naphthalenediols in Cosmetics
- High Performance Liquid Chromatography
ISSUED ON. FEBRUARY 06, 2018
IMPLEMENTED ON. SEPTEMBER 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
Introduction ... 4
1 Scope ... 5
2 Normative References ... 5
3 Principles ... 5
4 Reagents and Materials ... 6
5 Apparatus ... 6
6 Analytical Procedures ... 7
7 Results Calculation ... 8
8 Recovery Rate and Precision ... 9
9 Allowable Deviation ... 9
Appendix A (Informative) Information on Naphthalenediol Standard Substance
... 10
Appendix B (Informative) Liquid Chromatogram and Spectrogram of Four
Naphthalenediols Standard Substance Solutions ... 11
Appendix C (Informative) Confirmation Test ... 14
Determination of Four Naphthalenediols in Cosmetics
- High Performance Liquid Chromatography
1 Scope
This Standard specifies high performance liquid chromatography for the determination
of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-
naphthalenediol in cosmetics.
This Standard is applicable to the determination of 1,7-naphthalenediol, 2,3-
naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol in non-wax-based
cream, lotion, gel, water and powder cosmetics.
The method detection limit of this Standard. the method detection limit of four
naphthalenediols is 2.5mg/kg.
The method quantification limit of this Standard. the method quantification limit of four
naphthalenediols is 7.5mg/kg.
2 Normative References
The following documents are essential to the application of this document. For the
dated documents, only the versions with the dates indicated are applicable to this
document; for the undated documents, only the latest version (including all the
amendments) are applicable to this document.
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
3 Principles
The samples of cream, lotion, gel and water cosmetics shall be directly extracted by
95% ethanol; the samples of powder cosmetics shall be extracted by the mixture of
95% ethanol and 0.1% acetic acid solutions; the extracting solution shall be determined
by high-performance liquid chromatography after the filtering and centrifuging.
According to the retention time and spectrogram qualitative, use the external standard
quantitative method; if necessary, use liquid chromatography-mass
spectrometry/mass spectrometry to verify.
6 Analytical Procedures
6.1 Specimen processing
6.1.1 Cream, lotion and water specimens
Take 0.5g (accurate to 0.001g) of specimen; place it into 10mL stoppered colorimetric
tube; add 4mL of 95% ethanol (4.3); shake and mix on the vortex oscillator (5.3); then
perform ultrasonic extraction for 15min; cool off to the room temperature; use 95%
ethanol (4.3) to make constant volume to 5mL. Take 2mL of solution into the centrifuge
tube; centrifuge for 2min at 10000r/min; filter the supernatant through a filter membrane
(4.8) then determined by the high-performance liquid chromatography (5.1).
6.1.2 Powder specimen
Take 0.5g (accurate to 0.001g) of specimen; place it into 10mL stoppered colorimetric
tube; add 2mL of 95% ethanol (4.3); shake and mix on the vortex oscillator (5.3); then
add 2mL of 0.1% acetic acid solution (4.4); perform ultrasonic extraction for 15min;
cool off to the room temperature; use 95% ethanol (4.3) to make constant volume to
5mL. Take 2mL of solution into the centrifuge tube; centrifuge for 2min at 10000r/min;
filter the supernatant through a filter membrane (4.8) then determined by the high-
performance liquid chromatography (5.1).
6.2 Determination
6.2.1 Reference operating conditions of high-performance liquid chromatograph
The reference operating conditions of high-performance liquid chromatograph are as
follows.
a) Chromatographic column. C18 column, 5µm, 250mm×4.6mm (inner diameter), or
the equivalent;
b) Mobile phase. methanol (4.1) and 0.1% acetic acid solution (4.4), high-
performance liquid chromatograph gradient elution conditions are shown in Table
1;
c) Flow rate. 1.0mL/min;
d) Column temperature. 30°C;
e) Wavelength. 230nm;
f) Sampling-injecting volume. 20µL.
Where.
Xi – the content of the test composition in the specimen; in mg/kg;
ci – the mass concentration of the test composition in the specimen solution obtained
from the standard curve; in µg/mL;
c0 – the mass concentration of the test composition in the blank sample obtained from
the standard curve; in µg/mL;
V – the constant volume of the specimen solution, in mL;
m – specimen mass, in g;
f – dilution factor.
The results shall be retained two significant figures.
8 Recovery Rate and Precision
In the range of add concentration of 7.5mg/kg ~75mg/kg, the recovery rate is
80%~110%; the relative standard deviation is less than 10%.
9 Allowable Deviation
The absolute difference between two independent determinations obtained under
repeatability conditions shall not exceed 10% of the arithmetic mean.
Appendix C
(Informative)
Confirmation Test
C.1 Liquid chromatography reference conditions
The liquid chromatography reference conditions are as follows.
a) Chromatographic column. Luna C18(2), 150×2.0mm (inner diameter), 3µm; or the
equivalent;
b) Mobile phase. A – methanol; B – water; gradient elution. 0.0min~10.0min,
25%~65%A; 10.1min~30.0min, 65%A.
c) Flow rate. 150µL/min;
d) Column temperature. 25°C;
e) Sample-injecting volume. 10µL.
C.2 Mass spectrometry reference conditions
The mass spectrometry reference conditions are as follows.
a) Ion source. electrospray ion source;
b) Ionization mode. negative ion mode;
c) Ionization voltage. -4500V;
d) Atomizing gas pressure. 0.345MPa (50psi);
e) Air curtain gas pressure. 0.241MPa (35psi);
f) Auxiliary heating gas pressure. 0.483MPa (70psi);
g) Auxiliary gas temperature. 500°C;
h) Detection mode. Multiple Reaction Monitoring (MRM) mode. The mass
spectrometric analysis parameters of four naphthalenediols can refer to Table
C.1; the multiple reaction monitoring mass chromatograms of four
naphthalenediols can refer to Figure C.1.
C.3 Qualitative determination
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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