Method for measuring residual solvent in tetracycline hydrochloride bulk drug by utilizing headspace gas chromatography
A technology of headspace gas chromatography and tetracycline hydrochloride, which is applied in the direction of measuring devices, material separation, and analysis of materials, can solve the problems of decreased separation effect of chromatographic columns, interference of acetone and butanol analysis, and contamination of chromatographic columns, etc., to achieve the extension of chromatographic columns The effect of long life, less interference factors and large injection volume
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Embodiment 1
[0025] 1 Chromatographic conditions:
[0026] Chromatographic column: polyethylene glycol open capillary column; column temperature: 125°C; carrier gas: nitrogen; flow rate: 3 ml / min; inlet temperature: 200°C; detector: FID; detector temperature: 250°C; hydrogen Flow: 30 ml / min; air flow: 400 ml / min.
[0027] 2 Headspace conditions:
[0028] Headspace vial heating temperature: 80°C; headspace heating time: 25min; quantitative loop temperature: 105°C; transfer tube temperature: 125°C; quantitative loop volume: 1ml.
[0029] 3 Solution preparation:
[0030] (1) n-butanol stock solution: Accurately draw 1ml of n-butanol, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute it with water to the mark, and shake well.
[0031] (2) Acetone stock solution: Accurately absorb 1ml of acetone, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute to the mark with wat...
Embodiment 2
[0042] 1 Chromatographic conditions:
[0043] Chromatographic column: polyethylene glycol open capillary column; column temperature: 125°C; carrier gas: nitrogen; flow rate: 3 ml / min; inlet temperature: 200°C; detector: FID; detector temperature: 250°C; hydrogen Flow: 30 ml / min; air flow: 400 ml / min.
[0044] 2 Headspace conditions:
[0045] Headspace vial heating temperature: 80°C; headspace heating time: 25min; quantitative loop temperature: 105°C; transfer tube temperature: 125°C; quantitative loop volume: 1ml.
[0046] 3 Solution preparation:
[0047] (1) n-butanol stock solution: Accurately draw 1ml of n-butanol, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute it with water to the mark, and shake well.
[0048] (2) Acetone stock solution: Accurately absorb 1ml of acetone, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute to the mark with wat...
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