Agriculture, animal husbandry, fishing and forestry/feed testing

1 Scope This standard specifies the simultaneous determination of feed β- Liquid chromatography-mass spectrometry (LC-MS) method for the determination of agonists salbutamol, ractopamine, and clenbuterol hydrochloride. This standard is applicable to the determination of salbutamol, levodopa, and clenbuterol hydrochloride in formula feed, concentrated feed, and additive premixed feed. The detection limit for salbutamol, ractopamine, and clenbuterol hydrochloride in this standard is 0.01 mg/kg, and the quantitative limit is 0.05 mg/kg. 2 Normative references: The clauses in the following documents have become clauses of this standard through reference in this standard. For dated reference documents, all subsequent amendments (excluding corrected content) or revisions are not fully applicable to this standard. Therefore, all parties who have reached agreements based on this standard are encouraged to study whether the latest versions of these documents can be used. For undated references, the latest version applies to this standard. GB/T 6682 Specification and Test Methods for Analytical Laboratory Water (GB/T 6682-1992. neq 1SO 36961987) GB/T 14699.1 Feed - Sampling 3 Principles: The sample is extracted from a phosphoric acid methanol solution, purified with a solid-phase extraction column, and separated by a reverse phase Ca column gradient elution. The retention time and characteristic ions of the three substances are qualitatively and quantitatively determined using a mass spectrometry detector. Unless otherwise specified, all reagents and solutions used in this standard are analytical pure. Water meets the requirements of GB/T 6682 for secondary water use. 4.1 Acetonitrile: Chromatically pure. 4.2 Methanol. 4.3 Phosphate methanol extraction solution; Add 200 mL of water to 3.92 g of concentrated phosphoric acid, and then dilute to 1000 mL with methanol. 4.4 Ice acetic acid solution (2%): Dilute 10 mL of ice acetic acid with water to 500 mL. 4.5 Sodium sulfide solution (1 g/L): Weigh 0.250 g of sodium sulfide (NagS · 9H, O) and dissolve it in water, and bring to a constant volume of 250 mL. 4.6SPE small column eluent and eluent 4.6.1 Latent: Transfer 9 mL of concentrated hydrochloric acid to 1000 ml of water, shake well. 4.6.2 Eluent; Transfer 10 mL25% ammonia water into a 100 mL volumetric flask and bring to volume with methanol. 4.7 Mobile phase A liquid; Dissolve 3.65g of ammonium formate in 500 ml of deionized water, adjust the pH to 3.80 with formic acid. Solution B: acetonitrile, chromatographically pure. 4.8 Standard solution of salbutamol, ractopamine, and clenbuterol hydrochloride 4.8.1: Standard stock solution: Weigh 50 mg of salbutamol, ractopamine, and clenbuterol hydrochloride (with standard content of 98%) in a 50 mL brown volumetric flask, dissolve in methanol, and bring to volume to the mark. Store at 4 ℃ in the refrigerator for one month. 4.8.2 Standard working intermediate solution: Transfer 1 mL of standard stock solutions (4.8.1) of salbutamol, levodobactam, and clenbuterol hydrochloride into a 100 mL volumetric flask, and bring to volume with glacial acetic acid solution (4.4)

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