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GB/T 46279-2025: Determination of amprolium hydrochloride, ethopabate and sulfaquinoxaline in feeds
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GB/T 46279-2025: Determination of amprolium hydrochloride, ethopabate and sulfaquinoxaline in feeds

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ICS 65.120 CCSB46 National Standards of the People's Republic of China Replaces GB/T 8381.11-2005 Aminopropionate hydrochloride, ethoxymethyl benzoate and Determination of sulfaquinoline Published on 2025-08-29 Implemented on 2026-03-01 State Administration for Market Regulation The State Administration for Standardization issued a statement.

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 replaces GB/T 8381.11-2005 "Determination of Aminopropionate Hydrochloride in Feed by High Performance Liquid Chromatography". Compared with GB/T 8381.11-2005, apart from structural adjustments and editorial changes, the main technical changes are as follows. ---The scope of application and limit of detection have been changed, and a limit of quantitation has been added (see Chapter 1, Chapter 1 of the.2005 edition); ---The principles of high-performance liquid chromatography have been modified (see Chapter 4, Chapter 3 of the.2005 edition); ---The experimental procedures for high-performance liquid chromatography have been modified (see 4.5, Chapter 7 of the.2005 edition); ---The data processing for high performance liquid chromatography has been modified (see 4.6, Chapter 8 of the.2005 edition); ---A new chapter on "Liquid Chromatography-Tandem Mass Spectrometry" has been added (see Chapter 5). Please note that some content in this document may involve patents. The issuing organization of this document assumes no responsibility for identifying patents. This document was proposed and is under the jurisdiction of the National Technical Committee on Standardization of Feed Industry (SAC/TC76). This document was drafted by. Institute of Agricultural Quality Standards and Testing Technology, Chinese Academy of Agricultural Sciences; Shaanxi Provincial Animal Husbandry Technology Extension Station. Shaanxi Zhonghe Agricultural Inspection and Testing Co., Ltd., and Shaanxi Provincial Agricultural Inspection and Testing Center. The main drafters of this document are. Song Rong, Li Hong, Wei Shulin, Yan Hua, Xiao Hongnian, Yang Kun, Chao Juanjuan, Luo Yaxuan, Li Libei, Wang Suqin, and Zhang Hui. The release history of this document and the document it replaces is as follows. ---First published in.2005 as GB/T 8381.11-2005; ---This is the first revision. Aminopropionate hydrochloride, ethoxymethyl benzoate and Determination of sulfaquinoline 1.Scope This document describes high-performance liquid chromatography (HPLC) and liquid chromatography-tandem chromatography (LC-tandem chromatography) for the detection of aminopropionate hydrochloride, ethoxybenzone, and sulfaquinoxaline in feed. Mass spectrometry method. This document applies to ammonium hydrochloride in compound feed, concentrated feed, concentrate supplements, additive premixes, and mixed feed additives. Determination of propionyl, ethoxybenzoate and sulfaquinoline. In this document, the limit of detection (LOD) for amprolium hydrochloride using high-performance liquid chromatography (HPLC) is 10 mg/kg, and the limit of quantitation (LOQ) is 20 mg/kg; the detection limit for ethoxybenzoate is... The limit of expiratory volume (LOV) was 0.2 mg/kg, and the limit of quantitation (LOQ) was 0.4 mg/kg; the LAV of sulfaquine was 6 mg/kg, and the LOQ was 12 mg/kg. Liquid chromatography (LC) The detection limit for both spectrophotometers and tandem mass spectrometers was 0.02 mg/kg, and the quantitation limit was 0.05 mg/kg.

2 Normative references

The contents of the following documents, through normative references within the text, constitute essential provisions of this document. Dated citations are not included. For references to documents, only the version corresponding to that date applies to this document; for undated references, the latest version (including all amendments) applies. This document. GB/T 6682 Specifications and test methods for water used in analytical laboratories GB/T 20195 Preparation of animal feed samples 3.Terms and Definitions This document does not contain any terms or definitions that need to be defined. 4.High Performance Liquid Chromatography 4.1 Principle The analyte in the sample was extracted with methanol solution, defatted with n-hexane, purified by hydrophilic-lipophilic equilibrium solid-phase extraction column, and then separated by high performance liquid chromatography. The sample was measured using a UV detector in series with a fluorescence detector, and quantified using the external standard method. 4.2 Reagents or Materials Unless otherwise specified, use only analytical grade reagents. 4.2.1 Water. GB/T 6682, Grade I. 4.2.2 Methanol. chromatographic grade. 4.2.3 n-Hexane. 4.2.4 Extraction solution. a mixture of methanol (4.2.2) and water, V(methanol) V(water) = 4 1. 4.2.5 Phosphate buffer. Weigh 0.2g potassium dihydrogen phosphate and 13.68g dipotassium hydrogen phosphate trihydrate, dissolve in water and dilute to a final volume. Mix 1000mL thoroughly. 4.2.6 Eluent. Transfer 10 mL of methanol (4.2.2), dilute with water and bring the volume to 100 mL, and mix well. 4.2.7 Sodium heptanesulfonate solution (0.005 mol/L). Weigh 1 g of sodium heptanesulfonate into 800 mL of water, stir to dissolve, and add 6 mL of trichloroethylene (TCM) sodium sulfate solution. Ethylamine and 24 mL of glacial acetic acid were diluted with water to a final volume of 1000 mL and mixed thoroughly. 4.2.8 Reconstituted solution. a mixture of sodium heptanesulfonate solution (4.2.7) and methanol (4.2.2), V(sodium heptanesulfonate solution) V(methanol) = 1 1. 4.2.9 Standard stock solution (0.5 mg/mL). Accurately weigh amprolium hydrochloride (CAS No.. 137-88-2, purity not less than 98.0%), ethoxysulfate... Methylparaben (CAS No.. 59-06-3, purity not less than 98.0%) and sulfaquinoline (CAS No.. 59-40-5, purity not less than 98.0%). 50 mg of each solution (accurate to 0.01 mg) was placed in separate 100 mL volumetric flasks, dissolved and diluted to volume with methanol (4.2.2), and mixed well. The solution was then stored at -18℃. Stored at the following conditions, the shelf life of the standard stock solutions of amprolium hydrochloride and ethoxybenzoate is 9 months. The standard stock solution of sulfaquinoline is... The stock solution has a shelf life of 6 months. 4.2.10 Standard intermediate solution (100 μg/mL). Accurately transfer 10 mL of each of the standard stock solutions (4.2.9) into separate 50 mL volumetric flasks. Dilute with methanol (4.2.2) and bring to volume, then mix well. Store below -18℃; shelf life is 3 months. Ethoxybenzoate Standard Intermediate The solution was diluted 20 times with methanol (4.2.2) (5 μg/mL) before use. 4.2.11 Mixed Standard Series Solutions. Accurately transfer an appropriate amount of the intermediate standard solution (4.2.10) and prepare ampicillin hydrochloride using the reconstitution solution (4.2.8). The mass concentrations of porphyrin were 1 μg/mL, 2 μg/mL, 5 μg/mL, 10 μg/mL, 20 μg/mL and 50 μg/mL, and the mass of ethoxyamide benzyl ester was... The concentrations of sulfaquinoline were 0.05 μg/mL, 0.1 μg/mL, 0.25 μg/mL, 0.5 μg/mL, 1.0 μg/mL, and 2.5 μg/mL. A series of mixed standard solutions with concentrations of 0.6 μg/mL, 1.2 μg/mL, 3 μg/mL, 6 μg/mL, 12 μg/mL, and 30 μg/mL. (Prepared immediately before use) Prepared on the spot. 4.2.12 Solid phase extraction column. hydrophilic-lipophilic balanced column, 60mg/3mL, or equivalent. 4.2.13 Microporous filter membrane. 0.45μm, organic system. 4.3 Instruments and Equipment 4.3.1 Liquid Chromatograph. Equipped with an ultraviolet detector (or diode array detector) and a fluorescence detector, with the fluorescence detector connected in series with the ultraviolet detector. After the measuring device. 4.3.2 Analytical balance. accuracy 0.1mg, 0.01mg. 4.3.3 Vortex mixer. 4.3.4 Ultrasonic cleaner. 4.3.5 Centrifuge. The rotation speed shall not be less than 5000 r/min. 4.3.6 Solid phase extraction apparatus. 4.3.7 Nitrogen blowing device. 4.4 Samples Prepare samples according to GB/T 20195, at least.200g, crush them so that they all pass through a test sieve with a 0.425mm aperture, mix thoroughly, and load into... Store in a ground glass bottle for later use. 4.5 Test Procedure 4.5.1 Extraction Perform two parallel experiments. Weigh 2 g (m, accurate to 0.1 mg) of the sample into a 50 mL centrifuge tube and accurately add 25 mL of extraction solution. (4.2.4) Mix well, extract by sonication for 30 min (shaking once every 10 min during this period), centrifuge at 5000 r/min for 5 min, collect the supernatant and residue. Repeat the extraction once, combine the supernatants (V), and set aside. 4.5.2 Purification 4.5.2.1 Degreasing Transfer 8 mL of the stock solution (4.5.1), add 5 mL of n-hexane (4.2.3), vortex for 1 min, and centrifuge at 5000 rpm for 5 min. Accurately transfer... Take 5 mL (V1) of the lower layer solution (1 mL for additive premixed feed or mixed feed additive), and purge with nitrogen at 40°C until nearly Dry the sample, dissolve it in 3 mL of phosphate buffer (4.2.5) by vortexing, mix well, centrifuge at 5000 r/min for 5 min, and take all the supernatant for later use. 4.5.2.2 Solid-phase extraction The solid-phase extraction column (4.2.12) was activated sequentially with 3 mL of methanol (4.2.2), 3 mL of water, and 3 mL of phosphate buffer (4.2.5). The prepared solution... (4.5.2.1) Pass the entire column through the column, elute sequentially with 3 mL of water and 3 mL of eluent (4.2.6), dry under vacuum, elute with 3 mL of methanol (4.2.2), and collect. The eluent was dried nearly to dryness under nitrogen at 40°C. 1 mL (V2) of the reconstitution solution (4.2.8) was accurately added to dissolve the eluent, and the mixture was vortexed to mix. Microporous membrane. (4.2.13) Filtering, to be tested. 4.5.3 Measurement 4.5.3.1 Reference conditions for high performance liquid chromatography The reference conditions for high performance liquid chromatography are as follows. a) Chromatographic column. C18 column, 250 mm in length, 4.6 mm in inner diameter, 5 μm in particle size, or equivalent; b) Column temperature. 30℃; c) Mobile phase. Phase A is sodium heptanesulfonate solution (4.2.7), Phase B is methanol (4.2.2), and the gradient elution program is shown in Table 1; d) Flow rate. 1 mL/min; e) Injection volume. 20 μL; f) Ultraviolet detection wavelength. 267nm; g) Fluorescence detector. excitation wavelength 306nm, emission wavelength 350nm. Table 1 Gradient elution program time min Phase A (volume fraction) Phase B (volume fraction) 0.0 70 30 30.0 52 48 32.0 10 90 35.0 10 90 35.1 70 30 40.0 70 30 4.5.3.2 Determination of mixed standard series solutions and sample solutions Under optimal instrument conditions, the mixed standard series solution (4.2.11) and the sample solution (4.5.2.2) were respectively tested using ultraviolet light detection. A fluorescence detector (or diode array detector) was used to determine aminopropyl hydrochloride and sulfaquinoline, while a fluorescence detector was used to determine ethoxybenzoate. Mixed standards. The high-performance liquid chromatogram of the solution is shown in Appendix A. 4.5.3.3 Qualitative Qualitative analysis is based on retention time. The retention times of the analyte in the sample solution and the mixed standard series solutions (with equivalent mass concentrations) are consistent, indicating their relative... The deviation is within ±2.5%. 4.5.3.4 Quantitative analysis A standard curve should be plotted with the mass concentration of the analyte in the standard solution on the x-axis and the peak area on the y-axis. The correlation coefficient should not be lower than that of the standard curve. ...