T/NAASS 045-2022 Determination of residual acetone solvent in erythromycin thiocyanate by gas chromatography
T/NAASS 045-2022 Determination of residual acetone solvent in erythromycin thiocyanate by gas chromatography
Basic Information
Scope
Scope: This document specifies the gas chromatography method for the determination of acetone solvent residues in erythromycin thiocyanate. This document is applicable to the determination of acetone solvent residues in erythromycin thiocyanate; Main technical content: 3. Principle: The gas chromatograph equipped with a hydrogen flame ionization detector is used to separate, analyze, and determine the acetone solvent in erythromycin thiocyanate, with quantification performed using the external standard method. 4. Instruments and equipment 4.1 Gas chromatograph: Equipped with a hydrogen flame ionization detector and a headspace sampler. 4.2 Electronic balance: With a sensitivity of 0.0001 g. 4.3 Volumetric flasks: 25 mL, 50 mL. 4.4 Pipettes: 1 mL, 5 mL. 4.5 Headspace vials: 20 mL. 5. Reagents 5.1 Acetone (CH3COCH3), chromatograph-grade. 5.2 Reference solution: Accurately weigh 0.25 g of acetone (with a precision of 0.0001 g) and dissolve it in a 25 mL volumetric flask with water to the mark. Shake well, then accurately pipette 1.00 mL into a 50 mL volumetric flask and dilute with water to the mark. Shake well, and quickly and accurately pipette 5.00 mL into a 20 mL headspace vial and seal it as the reference solution. 6. Determination 6.1 Chromatographic conditions a) Chromatographic column: A capillary column filled with a 6% cyanopropyl phenyl-94% dimethyl siloxane (30 m × 530 μm, 3.0 μm). Unless otherwise specified, polarity-similar chromatographic columns with equivalent separation effects can be interchangeably used. b) Carrier gas: Nitrogen (purity > 99.999%). c) Carrier gas flow rate: 5 mL/min. d) Split ratio: 20:1. e) Column temperature: Initial temperature: 40 °C, held at this temperature for 5 min, then heated at a rate of 30 °C/min to 200 °C and maintained at 200 °C for 2.67 min. f) Injection port temperature: 200 °C. g) Detector: Hydrogen flame ionization detector (FID), temperature 250 °C. 6.2 Headspace sampler con