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GB 29688-2013: Determination of Chloramphenicol residues in milk by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Chloramphenicol residues in milk by Liquid Chromatography-tandem Mass Spectrometric method
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GB 29688-2013
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Basic data
| Standard ID | GB 29688-2013 (GB29688-2013) |
| Description (Translated English) | Determination of Chloramphenicol residues in milk by Liquid Chromatography-tandem Mass Spectrometric method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 12,156 |
| Quoted Standard | GB/T 6682; GB/T 1.1-2000 |
| Adopted Standard | GB/T 6682; GB/T 1.1-2000 |
| Regulation (derived from) | China Food & Drug Administration [2013] No. 234, November, 1, 2013 |
| Issuing agency(ies) | Ministry of Agriculture of the People's Republic of China, National Health and Family Planning Commission of the People's Republic of China |
| Summary | This standard specifies the Milk chloramphenicol residue detection sample preparation, liquid chromatography tandem mass spectrometry. This standard applies to milk the detection of chloramphenicol residues. |
GB 29688-2013: Determination of Chloramphenicol residues in milk by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Chloramphenicol residues in milk by Liquid Chromatography-tandem Mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Determination of chloramphenicol residues in milk
Liquid chromatography - tandem mass spectrometry
Published 2013-09-16
2014-01-01 implementation
Ministry of Agriculture, People's Republic of China
National Health and Family Planning Commission People's Republic of China released
National Food Safety Standard
Determination of chloramphenicol residues in milk
Liquid chromatography - tandem mass spectrometry
1 Scope
This standard specifies chloramphenicol Residues in Milk sample preparation and liquid chromatography - tandem mass spectrometry.
This standard applies to milk the detection of chloramphenicol residues.
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 6682-1992 specifications and test methods for water analysis laboratory
Principle 3
Chloramphenicol residues in a sample, extracted with ethyl acetate, hexane degreasing, C18, purified by liquid chromatography - tandem mass spectrometry, internal standard method
Quantitative.
4 Reagents and materials
The following reagents used, unless otherwise stated who were of analytical reagent; water as a water line with GB/T 6682 provisions.
Chloramphenicol 4.1 Standard. Content ≥97%.
4.2 Internal standard. Chloramphenicol deuterated standards. content 100μg/mL (as an internal standard stock standard solution).
4.3 Methanol. HPLC grade.
4.4 Acetonitrile. chromatographically pure.
4.5 ethyl acetate.
4.6 sodium chloride.
4.7 n-hexane.
4.8 C18 solid phase extraction column. 500mg/3mL, or equivalent person.
4.9 4% sodium chloride solution. Take sodium chloride 4g, dissolve and dilute to 100mL with water.
4.10 100μg/mL chloramphenicol standard stock solution. Weigh accurately chloramphenicol standard 10mg, in 100mL flask, dissolved in methanol and
Diluted to the mark, formulated at a concentration of 100μg/mL standard stock solution of chloramphenicol. -20 ℃ below, valid for one year.
4.11 100μg/L of chloramphenicol standard working solution. precise amount of 100μg/mL standard stock solution of chloramphenicol 100μL, in 100mL
Volumetric flask, dissolved in 50% acetonitrile and dilute to volume, formulated at a concentration of 100μg/L of the working standard solution. 2 ℃ ~ 8 ℃ preservation, effective
1 month.
4.12 20μg/L of chloramphenicol deuterated standard working solution. the precise amount of a deuterated standard 20 L of chloramphenicol, in 1000mL flask,
50% acetonitrile dissolve and dilute to volume, formulated at a concentration of 20μg/L chloramphenicol deuterated standard working solution. 2 ℃ ~ 8 ℃ preservation, effective
3 months.
5. Apparatus
5.1 liquid chromatography - tandem mass spectrometry. ion source distribution.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 Vortex.
5.5 oscillator.
5.6 tissue homogenizer.
5.7 refrigerated centrifuge.
5.8 rotary evaporator.
5.9 centrifuge tube. 50mL.
5.10 heart-shaped bottle. 50mL.
5.11 SPE.
5.12 Nitrogen blowing instrument.
5.13 filter. 0.22μm.
Preparation and Storage of sample 6
6.1 Preparation of the sample
An appropriate amount of fresh or frozen or blank test milk, mixed, and homogenized.
--- the test sample taken after homogenization, as the feed try.
--- blank sample taken after homogenization, as a blank sample.
--- blank sample taken after homogenization, adding a suitable concentration of the standard working solution, is added as a blank sample.
Save 6.2 sample
Or less at -20 ℃.
Determination Step 7
7.1 extract
Take Sample 10g ± 0.05g, in 50mL centrifuge tubes, add deuterated internal standard working solution 250 L of chloramphenicol, together with ethyl acetate 20mL,
Oscillation 15min, 6000r/min centrifugal 10min, the ethyl acetate layer was in heart-shaped flask. Coupled with 20mL ethyl acetate extraction was repeated a
Times, the two extracts were combined heart-shaped flask in a water bath at 45 ℃ rotary evaporated to dryness. The residue was dissolved with 4% sodium chloride solution 5mL, plus
5mL hexane oscillations 1min, standing layered hexane was discarded. Coupled with n-hexane 5mL, extraction was repeated once. Take subnatant
spare.
7.2 Purification
C18 column and washed with 5mL methanol and 5mL water activation, taking stock solution through the column, controlling the flow rate of 1 drop/(3s ~ 4s), 5mL water leaching
Washed, drained, washed with methanol 5mL, collecting eluate, blown dry with nitrogen at 50 ℃. With 50% acetonitrile and the residue was dissolved 1.0mL, vortex mixed
Uniform, membrane filtration, for liquid chromatography - tandem mass spectrometry.
7.3 Preparation of standard curve
The precise amount of 100μg/L of chloramphenicol standard working solution and 20μg/L of chloramphenicol deuterated amount of internal standard working solution, dilute with mobile phase
Release, formulated at a concentration of chloramphenicol 0.10,0.25,0.50,1.0,2.0,5.0μg/L, chloramphenicol deuterated concentration 5μg/L series of standard solutions
Solution for liquid chromatography - tandem mass spectrometer. A characteristic ion mass chromatogram peak area for the vertical axis, the standard solution at abscissa,
standard curve line. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 LC Conditions
7.4.1.1 Column. C18 (150mm × 2.1mm, particle size 5μm), or equivalent person.
7.4.1.2 Column temperature. 30 ℃.
7.4.1.3 flow rate. 0.2mL/min.
7.4.1.4 Injection volume. 20μL.
7.4.1.5 Run time. 8min.
7.4.1.6 Mobile phase. aqueous acetonitrile (50 50, volume ratio).
7.4.2 MS conditions
7.4.2.1 ionization mode. ESI.
7.4.2.2 Scan mode. negative ion scan.
7.4.2.3 Detection mode. multiple reaction monitoring.
7.4.2.4 ionization voltage. 2.8kV.
7.4.2.5 source temperature. 120 ℃.
7.4.2.6 atomizing temperature. 350 ℃.
7.4.2.7 Cone gas flow rate. 50L/h.
7.4.2.8 atomizing gas flow rate. 450L/h.
7.4.2.9 Data acquisition window. 8min.
7.4.2.10 dwell time. 0.3s.
7.4.2.11 qualitative and quantitative ion and the corresponding cone voltage and collision energy. see Table 1.
Table 1 chloramphenicol qualitative and quantitative Cone voltage of ion collision energy and
drug
Qualitative ion pair
m/z
Quantitative ion pair
m/z
Cone voltage
Collision voltage
Chloramphenicol (CAP)
321/151.6
321/256.8
321/151.6 30
Deuterated chloramphenicol
(D5-CAP)
325.8/156.6 325.8/156.6 30 15
7.4.3 Assay
Take a sample solution and standard solutions corresponding, for single or multi-point calibration, according to the internal standard peak area ratio calculation. Sample solution and control solution
Chloramphenicol broth and deuterated chloramphenicol response value should be within the linear range of the detection instrument. Ion in the sample solution and the relative abundance of labeled
Ion standard solution relative abundance ratio in accordance with Table 2. Tissue white standard solution and sample solution was added and the total ion selected ion
FIG flow Appendix A.
Table 2 sample ions in the solution relative abundance tolerance range
The relative abundance
Tolerance
> 50 ± 20
> 20 ~ 50 ± 25
> 10 ~ 20 ± 30
≤10 ± 50
7.5 Blank test
But without addition of the sample, the measurement step is performed in exactly the same operation in parallel.
8 and the result of the calculation expression
Calculating A321/151.6/A325.8/156.6 peak area ratio, the standard calibration curve.
From the standard curve equation.
As/A'is = a × cs/c'is b (1)
To obtain a and b, then
c =
c'is
Ais-
÷ b (2)
Chloramphenicol residues in a sample according to formula (3) is calculated.
X =
c × V
(3)
Where.
AS chloramphenicol --- the control solution peak area;
A'is --- internal control standard solution of chloramphenicol deuterated peak area;
--- CS control concentration deuterated internal standard solution of chloramphenicol, in units of nanograms per milliliter (ng/mL);
c'is --- chloramphenicol concentration control solution, in units of nanograms per milliliter (ng/mL);
C --- chloramphenicol test solution concentration unit nanograms per milliliter (ng/mL);
A --- chloramphenicol peak area of the sample;
Chloramphenicol deuterated standard peak area in the sample AIS ---;
X---- try feed for chloramphenicol residues in micrograms per kilogram (μg/kg);
V --- volume of the residue was dissolved in milliliters (mL);
m --- try supply feed mass in grams (g).
Note. The blank value should be subtracted from the results, expressed as the arithmetic mean of the measurement result measured parallel to three significant figures.
9 detection sensitivity, accuracy and precision
9.1 Sensitivity
This limit of detection is 0.01μg/kg, limit of quantification was 0.1μg/kg.
9.2 Accuracy
This method of adding 0.02μg/kg ~ 0.10μg/kg on recovery levels of 50% to 120%.
9.3 Precision
The relative standard deviation of the method ≤17%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
a)
b)
c)
d)
Figure A.1 chloramphenicol standard solution and wherein the total ion chromatogram mass ion (0.25μg/L)
a)
b)
Figure A.2 wherein milk sample blank ion mass chromatogram
c)
d)
Figure A.2 (continued)
a)
b)
c)
d)
Figure A.3 milk sample blank add chloramphenicol total ion chromatogram and mass characteristic ions (0.02μg/kg)
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