GB/T 18932.19-2003 PDF English
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Method for the determination of chloramphenicol residues in honey -- LC-MS-MS method
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GB/T 18932.19-2003: Method for the determination of chloramphenicol residues in honey -- LC-MS-MS method ---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT18932.19-2003
GB
ICS 67.180.10
X 31
National Standard
of the People’s Republic of China
Method for the determination of
chloramphenicol residues in honey -
LC-MS-MS method
Issued on. DECEMBER 26, 2003
Implemented on. JUNE 1, 2004
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine of the People’s Republic of China
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Principles... 4
4 Reagents & Materials... 5
5 Instruments... 5
6 Sample preparation and storage... 6
7 Determination steps... 6
8 Calculation of results... 8
9 Precision... 9
Foreword
This Part of GB/T18932 is modified on the basis of adopting the Canadian
Standard ACC-062-V1.0 "Method for the determination of chloramphenicol
residues in honey - LC-MS method". The main modified contents are as follows.
- Purification column is modified from C18 solid phase extraction column to
Oasis HLB solid phase extraction column;
- Eluent is modified from acetonitrile + water (3+7) to ethyl acetate;
- Single quadrupole mass-spectrometry detector is modified to tandem
quadrupole mass-spectrometry detector;
- Internal standard method is modified to the external standard method.
Appendix A and Appendix B of this Part are informative.
This Part was proposed by Qinhuangdao Entry - Exit Inspection and Quarantine
Bureau of the People's Republic of China.
This Part shall be under the jurisdiction of National Federation of Supply and
Marketing Cooperatives.
The drafting organization of this Part. Qinhuangdao Entry - Exit Inspection and
Quarantine Bureau of the People's Republic of China.
Main drafters of this Part. Pang Guofang, Cao Yanzhong, Zhang Jinjie, Jia
Guangqun, Fan Chunlin, Li Xuemin, Liu Yongming and Shi Yuqiu.
This Part was issued for the first time.
Method for the determination of chloramphenicol
residues in honey - LC-MS-MS method
1 Scope
This Part of GB/T 18932 specifies the method for the determination of
chloramphenicol residues in honey - LC-MS-MS method.
This Part is applicable to the determination of chloramphenicol residues in
honey.
The method detection limit of this Part. chloramphenicol is 0.10 μg/kg.
2 Normative References
The following standards contain the provisions which, through reference in this
Part of the GB/T18932, constitute the provisions of this Part. For dated
references, all subsequent amendments (excluding corrections) or revisions do
not apply to this Part. However, the parties who enter into agreement based on
this Part are encouraged to investigate whether the latest versions of these
standards are applicable. For undated reference documents, the latest versions
apply to this Part.
GB/T 6379 Precision of test methods - Determination of repeatability and
reproducibility for a standard test method by inter-laboratory tests (GB/T
6379-1986,neq IS05725.1981)
3 Principles
Use ethyl acetate to extract the sample. After the extract is concentrated,
dissolve it in water.
4 Reagents & Materials
4.1 Water. Grade-1 water specified by GB/T 6682.
4.2 Methanol. chromatographic pure.
4.3 Acetonitrile. chromatographic pure.
4.4 Ethyl acetate. chromatographic pure.
4.5 Acetonitrile + water (1+7). measure 20 mL of acetonitrile and mix it with 140
mL of water.
4.7 Chloramphenicol reference material. purity ≥ 99%.
4.8 Chloramphenicol standard stock solution. 0.1 mg/mL. Accurately weigh an
adequate amount of chloramphenicol reference material (4.7), and use
methanol to make 0.1 mg/mL standard stock solution. Store the stock solution
in the refrigerator at 4°C; it shall be used for two months.
5 Instruments
5.1 Liquid chromatography - tandem quadrupole mass spectrometer. equipped
with electrospray ionization source.
5.2 Analytical balances. 2 balances of which the sensitivity is 0.1 mg and 0.01
g respectively.
5.3 Automatic concentrator or equivalent.
5.4 Nitrogen blowing instrument.
5.10 Centrifuge.
5.11 Graduated centrifuge tube. 10 mL, the accuracy is 0.1 mL.
5.12 Pipette. 10 mL.
5.13 Centrifuge tube. 50 mL with stopper.
6 Sample preparation and storage
6.1 Sample preparation
Evenly stir the non-crystallized laboratory sample. For crystallized sample, in a
enclosed circumstance, place it in the water bath at not more than 60°C; warm
it; oscillate it till it is totally melted;
6.2 Sample storage
Store the sample at room temperature.
7 Determination steps
7.1 Extraction
Weigh 5 g of sample, accurate to 0.01 g. Place it into a 50 mL stoppered
centrifuge tube; add 5 mL of water. Quickly mix it in the liquid mixer for 1 min till
it is completely dissolved.
7.2 Purification
Pour the extract (7.1) into a liquid reservoir that is connected to Oasis HLB
column (4.6) in the lower. The solution flows through the Oasis HLB solid phase
extraction column at the flow rate ≤ 3 mL/min.
7.3 Determination
7.3.1 Liquid chromatography conditions
7.3.2 Mass-spectrometry conditions
321/194 -20
7.3.3 LC-MS-MS determination
Respectively inject the chloramphenicol standard working solutions (4.9) under
LC-MS-MS conditions. Take the peak area as ordinates, and take working
solution concentration (ng/mL) as abscissa; draw the seven-point standard
working curve.
7.4 Parallel test
Follow the previous steps to carry out the parallel test for the same sample.
7.5 Blank test
Follow the previous steps, except weighing the sample.
8 Calculation of results
The result is calculated according to equation (1).
9 Precision
The precision data in this Part is determined in accordance with the provisions
of GB/T 6379.The repeatability and reproducibility values are calculated in 95%
confidence.
9.1 Repeatability
Under conditions of repeatability, the content of chloramphenicol in honey is
between 0.19g/kg~4.0μg/kg. The absolute difference between two independent
test results obtained shall not exceed the repeatability limit (r). The repeatability
limit of this Part is calculated according to equation (2).
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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