GB/T 20744-2006 PDF English
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Method for the determination of metronidazole, ronidazole and dimetridazole residues in honey - LC-MS-MS method
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Basic data | Standard ID | GB/T 20744-2006 (GB/T20744-2006) | | Description (Translated English) | Method for the determination of metronidazole, ronidazole and dimetridazole residues in honey - LC-MS-MS method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | X04 | | Classification of International Standard | 67.050 | | Word Count Estimation | 9,922 | | Date of Issue | 2006-12-31 | | Date of Implementation | 2007-03-01 | | Quoted Standard | GB/T 6379.1; GB/T 6379.2 | | Regulation (derived from) | China National Standard Approval Announcement 2006 No.13 (Total No.100) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This standard specifies the honey metronidazole, ronidazole, dimetridazole residual liquid chromatography-tandem mass spectrometry. This standard applies to honey metronidazole, determination ronidazole dimetridazole residues. This standard method detection limit: metronidazole detection limit of 0. 1��g/kg, ronidazole and two metronidazole detection limits were 0. 2��g/kg. | GB/T 20744-2006: Method for the determination of metronidazole, ronidazole and dimetridazole 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/GBT20744-2006
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 67.050
X 04
Method for the determination of metronidazole,
ronidazole and dimetridazole residues in honey –
LC-MS-MS method
Issued on: DECEMBER 31, 2006
Implemented on: MARCH 01, 2007
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle ... 4
4 Reagents and materials ... 5
5 Instruments... 6
6 Sample preparation and preservation ... 6
7 Measurement step ... 7
8 Results calculation ... 9
9 Precision ... 9
Appendix A (Informative) Standard substance total ion chromatogram ... 11
Appendix B (Informative) Recovery ... 12
Foreword
The Appendix A and Appendix B of this Standard are informative.
This Standard was proposed by Qinhuangdao Entry - Exit Inspection and
Quarantine Bureau of the People's Republic of China.
This Standard shall be under the jurisdiction of the General Administration of
Quality Supervision, Inspection and Quarantine of People's Republic of China.
Drafting organizations of this Standard. Qinhuangdao Entry - Exit Inspection
and Quarantine Bureau of the People's Republic of China, Shandong
Agricultural University.
The main drafters of this Standard. Pang Guofang, Liu Yongming, Cao
Yanzhong, Fan Chunlin, Zhang Jinjie, Li Xuemin, Wu Yanping, Li Jin, Lian
Yujing, Lin Zhong.
This Standard is the first-time issued national standard.
6.2 Sample preservation
PRESERVE the sample under room temperature.
7 Measurement step
7.1 Extraction
WEIGH 10g of sample (accurate to 0.01g); PLACE it in a 50mL plugged glass
centrifuge tube; ADD 10 mL of water; MIX it uniformly on the liquid mixer; ADD
20mL of ethyl acetate; USE oscillator to vibrate it for 20min; MAKE it subject to
3000 r/min centrifugation for 5 min; TAKE the supernatant, MAKE it pass
through a cylindrical funnel containing 25 g of anhydrous sodium sulfate AND
reach into pear-shaped flask. USE 20 mL of ethyl acetate to extract it again,
MAKE it pass through the anhydrous sodium cylindrical funnel AND COMBINE
with the supernatant; USE a rotary evaporator to evaporate it at 45°C water
bath under reduced pressure to about 2mL; PREPARE for purification.
7.2 Purification
TRANSFER the aforementioned concentrate into the Carboxylic Acid solid-
phase extraction column; respectively USE 4 mL of ethyl acetate and 4mL of
acetonitrile to wash pear-shaped flask and extraction column; DISCARD all of
the effluent. Under the 65kPa negative pressure, REDUCE pressure and
EMPTY the extraction column for 2 min; USE 2 mL of eluent to conduct elution
at the flow rate ≤ 3 mL/min; COLLECT the elution solution into a 5mL scale
sample tube; USE eluent to make the volume reach to 2 mL; MAKE it pass
through 0.20μm filter membrane; PREPARE for the measurement by liquid
chromatography - tandem mass spectrometer.
7.3 Measurement
7.3.1 Liquid chromatography conditions
a) Chromatography column. Atlantis dC18, 3μm, 150 mm X 2.1 mm (inner
diameter) or the equivalent;
b) Mobile phase. acetonitrile + 0.1% formic acid solution (30 + 70);
c) Flow rate. 200μL/min;
d) Column temperature. 30°C;
e) Sample injection volume. 20μL.
7.3.2 MS conditions
Appendix B
(Informative)
Recovery
As for the adding concentration and average recovery of the metronidazole,
ronidazole, and dimetridazole in this method, see Table B.1.
Table B.1 Test data of metronidazole, ronidazole, and dimetridazole
adding concentration and average recovery
Drug name Adding concentration/(μg/kg) Mean recovery /(%)
Metronidazole
0.05 76.0
0.10 79.0
0.20 77.0
1.00 82.4
Ronidazole
0.10 69.5
0.20 78.5
0.40 73.9
2.00 71.7
Dimetridazole
0.10 75.6
0.20 74.9
0.40 75.4
2.00 81.7
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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