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GB 31656.3-2021: National food safety standard - Determination of norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin, oxolinic acid and flumequine residues in fishery products by high performance liquid chromatography
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National food safety standard - Determination of norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin, oxolinic acid and flumequine residues in fishery products by high performance liquid chromatography
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GB 31656.3-2021
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Basic data | Standard ID | GB 31656.3-2021 (GB31656.3-2021) | | Description (Translated English) | National food safety standard - Determination of norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin, oxolinic acid and flumequine residues in fishery products by high performance liquid chromatography | | Sector / Industry | National Standard | | Classification of Chinese Standard | X20 | | Word Count Estimation | 8,822 | | Issuing agency(ies) | National Health Commission of the People's Republic of China, State Administration for Market Regulation | GB 31656.3-2021: National food safety standard - Determination of norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin, oxolinic acid and flumequine residues in fishery products by high performance liquid chromatography
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Book national food safety standards
Norfloxacin, ciprofloxacin, enrofloxacin,
Determination of residual amounts of ofloxacin, quinic acid and flumequine
HPLC
National Standards of People's Republic of China
Released by the National Health Commission of the People's Republic of China
State Administration for Market Regulation
Ministry of Agriculture and Rural Affairs of the People's Republic of China
Foreword
This document complies with the provisions of GB/T 1:1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents"
Drafting:
This document is published for the first time:
National food safety standards
Norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin,
Determination of residual amounts of quinic acid and flumequine by high performance liquid chromatography
1 Scope
This document specifies the sample preparation for the detection of norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin, quinic acid, and flumequine residues in aquatic products
and high performance liquid chromatography determination methods:
This document is applicable to norfloxacin, ciprofloxacin, enrofloxacin, oxyfluoride in fish muscle tissue in aquatic products, and edible tissues of shrimp, crab, and shellfish:
Detection of residual amounts of floxacin, quinoacid and flumequine:
2 Normative reference documents
The contents of the following documents constitute essential provisions of this document through normative citations in the text: Among them, referenced documents with dates are only
The version corresponding to the date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to this document:
GB/T 6682 Specifications and test methods for water used in analytical laboratories
GB/T 30891-2014 Sampling specifications for aquatic products
3 Terms and definitions
There are no terms or definitions that need to be defined in this document:
4 Principles
Norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin, quinic acid, and flumequine remaining in the sample were extracted with acidified acetonitrile and removed with n-hexane:
Lipids were purified by C18 solid-phase extraction column, measured by liquid chromatography-fluorescence detection method, and quantified by external standard method:
5 Reagents and materials
Unless otherwise specified, all reagents are of analytical grade and the water is first-grade water that complies with GB/T 6682:
5:1 Reagents
5:1:1 Acetonitrile (CH₃CN): chromatographically pure:
5:1:2 Methanol (CH₃OH): chromatographically pure:
5:1:3 n-hexane (C₆H₁): chromatographically pure:
5:1:4 Hydrochloric acid (HCI),
5:1:5 Phosphoric acid (H₃PO₄):
5:1:6 Ammonia (NH₃·H₂O):
5:1:7 Sodium hydroxide (NaOH):
5:1:8 Sodium dihydrogen phosphate dihydrate (NaH₂PO₄·2H₂O):
5:1:9 Anhydrous sodium sulfate (Na₂SO₄):
5:1:10 Tetrabutylammonium bromide (C₁₆H₃₆BrN):
5:2 Standard products
Norfloxacin, ciprofloxacin, enrofloxacin, ofloxacin, quinic acid, and flumequine: content ≥ 98:0%, see Appendix A for details:
5:3 Solution preparation
5:3:1 Hydrochloric acid solution: Take 50mL of hydrochloric acid, add water to dilute to 100mL, and mix well:
5:3:2 Phosphoric acid solution: Take 1mL of phosphoric acid, add water to dilute to 10mL, and mix well:
5:3:3 Acidified acetonitrile solution: Take 250 mL of acetonitrile, add 2 mL of hydrochloric acid solution, and mix thoroughly:
5:3:4 Acetonitrile saturated n-hexane solution: Take:200 mL of n-hexane in a 250 mL separatory funnel, add an appropriate amount of acetonitrile, shake vigorously, and discard the acetonitrile layer after the distribution is balanced:
5:3:5 0:1mol/L hydrochloric acid solution: Take 9mL of hydrochloric acid and dilute it with water to 1000mL:
5:3:6 0:1mol/L sodium hydroxide solution: Take 4g of sodium hydroxide, dissolve it in water and dilute it to 1000mL:
5:3:7 0:05mol/L phosphate buffer solution: Take 1:56g of sodium dihydrogen phosphate dihydrate, add 79mL of 0:1mol/L sodium hydroxide solution to dissolve, and dilute to:200mL with water:
5:3:8 0:01mol/L tetrabutylammonium bromide solution (pH 3:0): Take 3:22g of tetrabutylammonium bromide, add 900 mL of water to dissolve, adjust the pH to 3:0 with phosphoric acid solution, and use water Dilute to 1000mL:
5:3:9 Eluent: Take 25 mL of ammonia water and dilute it with methanol to 100 mL:
5:4 Preparation of standard solution
5:4:1 Standard stock solution of norfloxacin and ofloxacin (100 μg/mL): Take about 10 mg each of norfloxacin and ofloxacin, weigh it accurately, and add 10 mL of 0:1 mol/L hydrochloric acid solution: Dissolve, dilute with acetonitrile to a 100mL brown volumetric flask, shake well, and get it: Store below 4°C in the dark, and is valid for 3 months:
5:4:2 Standard stock solution of ciprofloxacin and enrofloxacin (100 μg/mL): Take about 10 mg each of ciprofloxacin hydrochloride and enrofloxacin, weigh it accurately, dissolve it in methanol and dilute it to a constant volume: Put it in a 100mL brown volumetric flask, shake well, and it is ready: Store it below 4℃ in the dark, and it is valid for 3 months:
5:4:3 Standard stock solution of quinoacid and flumequine (100 μg/mL): Take about 10 mg each of quinoacid and flumequine, weigh it accurately, dissolve it with 10 mL of 0:1 mol/L sodium hydroxide solution, and add Dilute acetonitrile to a 100mL brown volumetric flask, shake well, and get it: Store below 4°C in the dark, and is valid for 3 months:
5:4:4 Mixed standard working solution (10 μg/mL): Precisely measure norfloxacin and ofloxacin standard stock solutions, ciprofloxacin and enrofloxacin standard stock solutions, quinic acid, and flumequine Put 1 mL of each standard stock solution into a 10 mL brown volumetric flask, dilute to volume with mobile phase A, shake well, and prepare:
Mix the standard working solution with a concentration of 10 μg/mL: Store in a dark place below 4°C and has a validity period of 1 month:
5:5 Materials
C18 solid phase extraction column: 500mg/3mL, or equivalent:
6 Instruments and equipment
6:1 High performance liquid chromatograph: equipped with fluorescence detector:
6:2 Analytical balance: sensitivity 0:00001g and 0:01g:
6:3 Nitrogen blowing instrument:
6:4 Ultrasonic oscillator:
6:5 Homogenizer: 15000r/min:
6:6 Centrifuge: 4000r/min:
6:7 Nylon microporous filter membrane: 0:22μm:
6:8 Pear-shaped bottle: 100mL:
6:9 Separating funnel: 250mL:
6:10 Rotary evaporator:
6:11 Separating funnel shaker:
7 Preparation and preservation of specimens
7:1 Preparation of specimens
Take an appropriate amount of fresh or thawed blank or test tissue and prepare samples according to the requirements of Appendix B in GB/T 30891-2014:
a) Take the homogenized test sample as the test sample;
b) Take the homogenized blank sample as the blank sample;
c) Take the homogenized blank sample, add standard working solution of appropriate concentration, and add the sample as a blank:
7:2 Storage of specimens
Store below -18℃ and conduct analysis and testing within 3 months:
8 Measurement steps
8:1 Extraction
Weigh 5g of the sample (accurate to ±0:02g), add 20mL of acidified acetonitrile solution and 10g of anhydrous sodium sulfate, and homogenize at high speed for 1 to 2 minutes:
Centrifuge at 3000 r/min for 5 minutes, take the supernatant to a separatory funnel, use 20 mL of acidified acetonitrile solution, clean the blade and dissolve the precipitate, repeat the extraction twice, and combine the supernatants: Add 60 mL of acetonitrile-saturated n-hexane solution and set the separatory funnel: Shake on a shaker (150r/min) for 20 minutes, let it stand, remove the acetonitrile layer and place it in a pear-shaped bottle, and rotary evaporate it to dryness at 40°C: Add 4 mL of phosphate buffer, ultrasonic oscillate for 1 min, let it stand for 30 s, and transfer the solution to
15 mL centrifuge tube: Repeat the extraction of the residue 2 times, transfer the solution to the same centrifuge tube, combine the residue solution 3 times, and centrifuge at 3000 r/min:
Incubate for 5 minutes, take the supernatant and set aside:
8:2 Purification
Take a C18 solid-phase extraction column and activate it with 3 mL each of methanol, water, and phosphate buffer: Pass the above reserve solution through the column, and control the flow rate to
1 drop per second: Elute with 3 mL of water, drain, add 5 mL of eluent, collect the eluate, blow dry with nitrogen at 50°C, add 1:0 mL of mobile phase A to dissolve:
Pass through a 0:22 μm microporous filter membrane and measure by high performance liquid chromatography:
8:3 Preparation of standard curve
Precisely measure appropriate amounts of mixed standard working solutions, and dilute them with mobile phase A to concentrations of 10ng/mL, 50ng/mL, and 100ng/mL respectively:
A series of standard solutions of mL, 500ng/mL, 1000ng/mL, and:2000ng/mL are provided for high-performance liquid chromatography analysis; ready for use: Use peak area as the ordinate and concentration as the abscissa to create a standard curve:
8:4 Determination
8:4:1 Chromatographic conditions
a) Chromatographic column: C18 chromatographic column (150mm×4:6mm, 5μm), or equivalent;
b) Mobile phase: A is 0:01mol/L tetrabutylammonium bromide solution-acetonitrile (94:6, V/V), B is acetonitrile, and the gradient elution conditions are shown in Table 1;
c) Flow rate: 0:9mL/min;
d) Column temperature: 35℃;
e) Injection volume: 10μL;
f) Detection wavelength: see Table 2 for the time program:
8:4:2 Determination method
Take the sample solution and standard solution, perform single-point or multi-point calibration, and quantify the chromatographic peak area according to the external standard method:
The peak area of the standard drug should be within the linear range of instrument detection: Under the above chromatographic conditions, the chromatogram of the mixed standard solution is shown in Appendix B:
8:5 Blank test
Take a blank sample and perform parallel operations using the same measurement steps except that no standard solution is added:
9 Calculation and presentation of results
The residual amount of the drug to be tested in the sample is calculated according to the standard curve or formula (1):
10 Method sensitivity, accuracy and precision
10:1 Sensitivity
The detection limit of norfloxacin, ciprofloxacin, enrofloxacin, and ofloxacin in this method is 2:5 μg/kg, and the detection limit of quinic acid and flumequine is
The limit of quantification of norfloxacin, ciprofloxacin, enrofloxacin and ofloxacin is 5μg/kg, and the limit of quantification of quinic acid and flumequine is 5μg/kg:
10μg/kg:
10:2 Accuracy
The recovery rate of norfloxacin, ciprofloxacin, enrofloxacin and ofloxacin at 5μg/kg~100μg/kg is 70%~
120%; the recovery rate of quinic acid and flumequine at the added concentration of 10 μg/kg~100 μg/kg is 70%~120%:
10:3 Precision
The intra-batch relative standard deviation of this method is ≤15%, and the inter-batch relative standard deviation is ≤15%:
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