GB/T 18932.24-2005 PDF in English
GB/T 18932.24-2005 (GB/T18932.24-2005, GBT 18932.24-2005, GBT18932.24-2005)
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Method for the determination of the metabolite residues of furaltadon, nitrofurazone, nitrofurantoin and furazolidone in honey -- Liquid chromatography-tandem mass spectrometry method
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Standards related to (historical): GB/T 18932.24-2005
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GB/T 18932.24-2005: PDF in English (GBT 18932.24-2005) GB/T 18932.24-2005
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.180.10
X 31
Method for the determination of the metabolite
residues of furaltadon, nitrofurazone, nitrofurantoin
and furazolidone in honey - Liquid chromatography -
tandem mass spectrometry method
ISSUED ON. FEBRUARY 04, 2005
IMPLEMENTED ON. AUGUST 01, 2005
Issued by.
General Administration of Quality Supervision, Inspection
and Quarantine of the People’s Republic of China;
Standardization Administration of the People’s Republic of
China.
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 ... 7
7 Determination steps ... 7
8 Result calculation ... 10
9 Precision ... 11
Annex A ... 13
Annex B ... 14
Foreword
Annex A and Annex B in this Part of GB/T 18932 are informative.
This Part was proposed by Qinhuangdao Entry-exit Inspection and Quarantine Bureau
of the People’s Republic of China.
The Part shall be under the jurisdiction of China Supply and Marketing Cooperatives.
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, Zhang Jinjie, Cao Yanzhong, Guo Tongtong;
Fan Chunlin, Li Xuemin, Liu Yongming, Cao Yaping.
This Part is first-time released national standard.
Method for the determination of the metabolite residues of
furaltadon, nitrofurazone, nitrofurantoin and furazolidone
in honey - Liquid chromatography - tandem mass
spectrometry method
1 Scope
This Part of GB/T 18932 specifies the liquid chromatography - tandem mass
spectrometry determination method for the metabolite residues of 5-methylmorpholine-
3-amino-2-yl alkyl ketones in furaltadon, semicarbazide in nitrofurazone, 1-amino-2-
hydantoin in nitrofurantoin and 3-amino-2-yl alkyl ketones in furazolidone in honey.
This Part applies to the determination of the residues of 5-methylmorpholine-3-amino-
2-yl alkyl ketones, semicarbazide, 1-amino-2-hydantoin and 3-amino-2-yl alkyl ketones
in honey.
The detection limit of the method in this Part. 0.2μg/kg for 5-methylmorpholine-3-
amino-2-yl alkyl ketones and 3-amino-2-yl alkyl ketones; 0.5μg/kg for semicarbazide
and 1-amino-2-hydantoin.
2 Normative references
The provisions in following documents become the provisions of this Part through
reference in this Part of GB/T 18932. For dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this Part, however,
parties who reach an agreement based on this Part are encouraged to study if the
latest versions of these documents are applicable. For undated references, the latest
edition of the referenced document applies.
GB/T 6379 Precision of test methods - Determination of repeatability and
reproducibility for a standard test method by interlaboratory tests (GB/T 6379-1986,
neq ISO 5725.1981)
GB/T 6682 Water for analytical laboratory use - Specification and test methods
(GB/T 6682-1992, neq ISO 3696.1987)
3 Principle
column moist.
4.16 0.45μm filter membrane.
4.17 5-methylmorpholine-3-amino-2-yl alkyl ketones, semicarbazide, 1-amino-2-
hydantoin and 3-amino-2-yl alkyl ketones reference material. Purity ≥99%.
4.18 5-methylmorpholin-3-amino-2-yl alkyl ketone, semicarbazide, 1-amino-2-
hydantoin and 3-amino-2-yl alkyl ketones standard stock solution. 1.0mg/mL. WEIGH
appropriate amount of the reference material of four kinds of nitrofuran metabolites
(4.17); USE methanol to prepare 1.0mg/mL standard stock solution. The stock solution
shall be stored in a freezer of -18°C, away from lights; the storage period is three
months.
4.19 5-methylmorpholin-3-amino-2-yl alkyl ketone, semicarbazide, 1-amino-2-
hydantoin and 3-amino-2-yl alkyl ketone mixed standard working solution. 1.0μg/mL.
PIPETTE appropriate amount of the standard stock solution of four kinds of nitrofuran
metabolites (4.18); USE methanol to prepare 1.0μg/mL mixed standard working
solution. The standard working solution shall be stored in a freezer of -18°C, away from
lights; the storage period is three months; RESUME to room temperature before use.
4.20 5-methylmorpholin-3-amino-2-yl alkyl ketone, semicarbazide, 1-amino-2-
hydantoin and 3-amino-2-yl alkyl ketone mixed matrix standard calibration solution.
WEIGH 7 honey blank samples (the sample weight is 4g) in 50mL brown centrifuge
tubes; ADD appropriate amount of the mixed standard working solution of four kinds
of nitrofuran metabolites (4.19) in 6 blank samples respectively; OPERATE
synchronously in accordance with the sample operation procedures. So that the
concentration of 5-methylmorpholin-3-amino-2-yl alkyl ketone and 3-amino-2-yl alkyl
ketones are respectively 0ng/mL, 0.5ng/mL, 1.0ng/mL, 2.0ng/mL, 5.0ng/mL,
10.0ng/mL and 20.0ng/mL; the concentration of semicarbazide and 1-amino-2-
hydantoin are respectively 0ng/mL, 1.0ng/mL, 2.0ng/mL, 5.0ng/mL, 10.0ng/mL,
20.0ng/mL and 50.0ng/mL in the final sample solutions; take them as matrix standard
calibration solution. This matrix standard calibration solution is prepared when it is to
be used.
5 Instruments
5.1 Liquid chromatography - tandem quadrupole mass spectrometer, equipped with
electrospray ion source.
5.2 Analytical balances. 2 balances with sensitivity of 0.1mg and 0.01g respectively.
5.3 Liquid mixer.
5.4 Solid phase extraction device.
to wash solid phase extraction column; DISCARD all of the effluent. USE a vacuum
pump (5.7) to drain the Oasis HLB solid phase extraction column for 10min at 65kPa
negative pressure. USE 4mL of ethyl acetate (4.3) to elute the analyte; COLLECT the
eluent in a 25mL brown centrifuge tube; DRY in a nitrogen blowing instrument (5.5) by
40°C water bath; USE 1mL of sample constant-volume solution (4.14) to dilute to
constant volume. After the constant-volume solution is mixed, MAKE it pass through
the 0.45μm filter membrane (4.16); the filtrate is used for determination by liquid
chromatography - tandem mass spectrometry.
7.3 Determination
7.3.1 Liquid chromatography conditions
a) Chromatographic column. ZORBAX SB-C18, 3.5μm, 150mm × 2.1mm
(diameter) or the equivalent;
b) Column temperature. 30°C;
c) Injection volume. 40μL;
d) Mobile phase and flow rate are shown in Table 1.
Table 1 Liquid chromatography gradient elution conditions
Time/min Flow rate/(μL/min) 0.4% acetic acid aqueous solution/(%) Acetonitrile/(%)
0.00 200 70 30
3.00 200 70 30
3.01 200 20 80
8.00 200 20 80
8.01 200 70 30
15.00 200 70 30
7.3.2 Mass spectrometer conditions
a) Ion source. electrospray ion source (ESI);
b) Scan mode. positive ion scan;
c) Detection method. multiple reaction monitoring (MRM);
d) Electrospray ionization voltage (IS). 5500V;
e) Nebulizer (NEB) pressure. 0.076MPa;
f) Curtain air (CUR) pressure. 0.069MPa;
g) Collision air (CAD) pressure. 0.030MPa;
(μg/kg);
c - Concentration of the tested component solution, obtained from standard
working curve, in nanograms per milliliter (ng/mL);
V - Final constant volume of the sample solution, in milliliters (mL);
m - Mass of the final sample represented by sample solution, in grams (g).
Note. the blank values shall be deducted from the calculation results.
9 Precision
The precision data in this Part are determined in accordance with the specifications of
GB/T 6379. The repeatability and reproducibility values are calculated by 95%
confidence.
9.1 Repeatability
Under repeatability conditions, the absolute difference between two independent test
results obtained shall not exceed the repeatability limit (r). The content range and
repeatability equation of four kinds of nitrofuran metabolites in honey are shown in
Table 4.
If the difference exceeds the repeatability limit, it shall abandon the test results and re-
complete the determination of two single tests.
9.2 Reproducibility
Under reproducibility conditions, the absolute difference between two independent test
results obtained shall not exceed reproducibility limit (R). The content range and
reproducibility equation of four kinds of nitrofuran metabolites in honey are shown in
Table 4.
Table 4 Content range AND repeatability and reproducibility equations
Name of nitrofuran
meta...
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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