Method for detecting content of propargyl alcohol in phosphonomycin-1-phenethylamine salt by headspace gas chromatography
A kind of headspace gas chromatography, levophosphine dexamine salt technology, applied in the field of drug analysis
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Embodiment 1
[0024] (1) Instrument conditions:
[0025] Chromatographic column: DB-1301 30m×0.53mm×1μm (capillary packed column filled with 6% cyanopropyl and 94% methylpolysiloxane, manufacturer: Agilent);
[0026] Detector: flame ionization detector;
[0027] Carrier gas: N2;
[0028] Column temperature: The initial column temperature of the instrument should be 70°C for 5 minutes, then raise the temperature to 115°C at 10°C / min and hold for 1 minute, then raise the temperature to 200°C at 50°C / min and hold for 2 minutes;
[0029] Headspace bottle press time is 0.05min;
[0030] The column flow rate is 4ml / min;
[0031] Injection volume: 1ml;
[0032] (2) Preparation of system adaptability solution:
[0033] Accurately weigh 0.5052 g of propynyl alcohol in a 100 ml volumetric flask, and add water to make up to the mark. Then accurately draw 1.0ml of this solution into a 200ml volumetric flask, and add water to make up to the mark.
[0034] (3) Preparation of the test solution:
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Embodiment 2
[0047] Establishment of methodology
[0048] 1 specificity test
[0049] 1.1 Preparation of system suitability solution:
[0050] Accurately weigh an appropriate amount of propynyl alcohol, add water to dissolve and dilute;
[0051] 1.2 Precisely measure 10ml of solvent water and system suitability test solution into a 20ml headspace bottle and seal it immediately; record the chromatogram, which shows that there is no interference from solvent water.
[0052] 2 linear range
[0053] Accurately weigh 0.5 g of propynyl alcohol in a 100 ml volumetric flask, add water to make up to the mark. Then accurately draw 1.0ml of this solution into a 200ml volumetric flask, and add water to make up to the mark.
[0054] Precisely measure 0.1, 0.25, 0.5, 1.0ml, and 1.2ml of the above solution into five 200ml volumetric flasks, dilute with water to the mark, shake well, precisely measure 10ml of the above solution into a 20ml headspace bottle, and seal it immediately; Record the chromat...
Embodiment 3
[0070] 1. Selection of chromatographic column
[0071] The chromatographic column filled with 6% cyanopropyl and 94% methyl polysiloxane has the best peak shape of propargyl alcohol, the best tailing factor, the best repeatability and durability of the method.
[0072] 2. Selection of headspace bottle press time
[0073] Adjust the headspace bottle pressure time to 0.05min.
[0074] 3. Selection of instrument column temperature
[0075] The initial column temperature of the instrument should be 70°C and kept for 5 minutes to make the main peak come out, then increase the temperature at 10°C / min to 115°C and hold for 1 minute, then increase the temperature to 200°C at 50°C / min and keep for 2 minutes to remove all impurity peaks.
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Application Information
- IPC
- G01N30/02
- Inventors
- 辛潇; 邵冬梅