CN104655739A - Method of measuring the content of propanol in tail gas from fermentation of erythromycin through headspace gas chromatography - Google Patents
Method of measuring the content of propanol in tail gas from fermentation of erythromycin through headspace gas chromatography Download PDFInfo
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- CN104655739A CN104655739A CN201310585508.8A CN201310585508A CN104655739A CN 104655739 A CN104655739 A CN 104655739A CN 201310585508 A CN201310585508 A CN 201310585508A CN 104655739 A CN104655739 A CN 104655739A
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Abstract
The invention relates to a method of measuring the content of propanol in tail gas from fermentation of erythromycin through headspace gas chromatography, in which the headspace gas chromatography is employed. The method includes steps of: (1) feeding the tail gas from fermentation into a headspace bottle through a guide pipe; (2) heating the tail gas at 90 DEG C; and (3) feeding 1ml of the heated tail gas into a gas chromatograph for performing measurement. The method is low in equipment requirement, is quick in operation and is high in accuracy.
Description
Technical field
The invention belongs to biological raw material detection technique field, particularly relate to the method for alcohol content in a kind of Headspace Gas Chromatography abomacetin fermentation tail gas.
Background technology
Erythromycin (erythromycin, Er) be macrolide antibiotics, be by red saccharopolyspora (Saccharopolyspora erythraea) through three grade fermemtation, the secondary metabolite of synthesis, is mainly used in suppressing gram-positive bacteria clinically.Earlier fermentation can add prerequisite material n-propanol in fermentation liquor, and object improves erythromycin in fermentation liquor to tire.The n-propanol part added is utilized by bacterium, and a part is along with air volatilization.In order to investigate the relation between n-propanol addition, microorganism utilization, volatile quantity, must detect n-propanol content in fermentation tail gas.
Summary of the invention
Object of the present invention is just to set up a kind of method that can measure alcohol content in abomacetin fermentation tail gas.
Technical scheme taked for achieving the above object is: preparation of samples: by fermentation tail gas by tubule, imports bottom 20ml ml headspace bottle, and keeps 10 ~ 15min, take out conduit immediately, jump a queue, and clamp with aluminium lid.Contrast prepares: pipette propyl alcohol reference substance 0.5 ~ 1 μ l with micropipettor, put in 20ml ml headspace bottle, jump a queue, and clamp with aluminium lid.Operation: get the ml headspace bottle that sample and contrast are housed, put in head-space sampler, detect by headspace gas chromatography.Head-space sampler condition is: sample bottle heating-up temperature is 90 DEG C, heat time 20 ~ 30min, quantitative loop temperature 100 DEG C, transfer tube temperature 110 DEG C, and sample size is 1ml.GC conditions is: chromatographic column: PEG 20000,0.53mm × 30m, thickness 1.0 μm.Column temperature 110 DEG C, runs 15min.Carrier gas is nitrogen, flow velocity 3ml/min.
Embodiment
1 head space condition: sample bottle heating-up temperature is 90 DEG C, heat time 20 ~ 30min, quantitative loop temperature 100 DEG C, transfer tube temperature 110 DEG C, sample size is 1ml.
2 chromatographic conditions:
Chromatographic column: PEG 20000,0.53mm × 30m, thickness 1.0 μm; Carrier gas is nitrogen, flow velocity 3ml/min.Column temperature 110 DEG C, run 15min, injector temperature is 150 DEG C
3 preparation of samples: by fermentation liquor tail gas by tubule, import bottom 20ml ml headspace bottle, and keep 10 ~ 15min, take out conduit immediately, jump a queue, and clamp with aluminium lid.Contrast prepares: pipette propyl alcohol reference substance 0.5 ~ 1 μ l with micropipettor, put in 20ml ml headspace bottle, jump a queue, and clamp with aluminium lid.
4 measure: get the ml headspace bottle that sample and contrast are housed, put in head-space sampler, detect by headspace gas chromatography.
Embodiment 1,
1 head space condition: sample bottle heating-up temperature is 90 DEG C, heat time 20min, quantitative loop temperature 100 DEG C, transfer tube temperature 110 DEG C, sample size is 1ml.
2 chromatographic conditions:
Chromatographic column: HP-INNOwax 30m × 0.53mm, thickness 1.0 μm; Carrier gas is nitrogen, flow velocity 3ml/min.Column temperature 110 DEG C, run 15min, injector temperature is 150 DEG C.
3 preparation of samples: by fermentation liquor tail gas by tubule, import bottom 20ml ml headspace bottle, keep 10min, take out conduit immediately, jump a queue, and clamp with aluminium lid.Contrast prepares: pipette propyl alcohol reference substance 0.5 μ l with micropipettor, put in 20ml ml headspace bottle, jump a queue, and clamp with aluminium lid.
3 measure:
Get the ml headspace bottle that sample and contrast are housed, put in head-space sampler, detect by headspace gas chromatography.
Test sample lot number: 130721, test sample is originated: Qiyuan Pharmaceutical Co., Ltd., Ningxia
Measurement result: 0.18ppm
Embodiment 2
1 head space condition: sample bottle heating-up temperature is 90 DEG C, heat time 25min, quantitative loop temperature 100 DEG C, transfer tube temperature 110 DEG C, sample size is 1ml.
2 chromatographic conditions:
Chromatographic column: HP-INNOwax 30m × 0.53mm, thickness 1.0 μm; Carrier gas is nitrogen, flow velocity 3ml/min.Column temperature 110 DEG C, run 15min, injector temperature is 150 DEG C.
3 preparation of samples: by fermentation liquor tail gas by tubule, import bottom 20ml ml headspace bottle, keep 12min, take out conduit immediately, jump a queue, and clamp with aluminium lid.Contrast prepares: pipette propyl alcohol reference substance 0.8 μ l with micropipettor, put in 20ml ml headspace bottle, jump a queue, and clamp with aluminium lid.
3 measure:
Get the ml headspace bottle that sample and contrast are housed, put in head-space sampler, detect by headspace gas chromatography.
Test sample lot number: 130722, test sample is originated: Qiyuan Pharmaceutical Co., Ltd., Ningxia
Measurement result: 0.23ppm
Embodiment 3
1 head space condition: sample bottle heating-up temperature is 90 DEG C, heat time 30min, quantitative loop temperature 100 DEG C, transfer tube temperature 110 DEG C, sample size is 1ml.
2 chromatographic conditions:
Chromatographic column: HP-INNOwax 30m × 0.53mm, thickness 1.0 μm; Carrier gas is nitrogen, flow velocity 3ml/min.Column temperature 110 DEG C, run 15min, injector temperature is 150 DEG C.
3 preparation of samples: by fermentation liquor tail gas by tubule, import bottom 20ml ml headspace bottle, and keep 15min, take out conduit immediately, jump a queue, and clamp with aluminium lid.Contrast prepares: pipette propyl alcohol reference substance 1 μ l with micropipettor, put in 20ml ml headspace bottle, jump a queue, and clamp with aluminium lid.
3 measure:
Get the ml headspace bottle that sample and contrast are housed, put in head-space sampler, detect by headspace gas chromatography.
Test sample lot number: 130723, test sample is originated: Qiyuan Pharmaceutical Co., Ltd., Ningxia
Measurement result: 0.20ppm.
Claims (3)
1. the method for alcohol content in a Headspace Gas Chromatography abomacetin fermentation tail gas, it is characterized in that: fermentation liquor tail gas is passed through tubule, import bottom 20ml ml headspace bottle, and keep 10 ~ 15min, get the ml headspace bottle that sample and contrast are housed, put in head-space sampler, detect by headspace gas chromatography.
2. according to the method for alcohol content in Headspace Gas Chromatography abomacetin fermentation tail gas according to claim 1, it is characterized in that fermentation liquor tail gas imports after bottom ml headspace bottle, keep 10 ~ 15min, sample bottle heating-up temperature is 90 DEG C, heat time 20 ~ 30min, quantitative loop temperature 100 DEG C, transfer tube temperature 110 DEG C, sample size is 1ml.
3. according to the method for alcohol content in Headspace Gas Chromatography abomacetin fermentation tail gas according to claim 1, it is characterized in that the chromatographic condition of above-mentioned vapor-phase chromatography is: chromatographic column: PEG 20000,0.53mm × 30m, thickness 1 μm, column temperature: 110 DEG C, run 15min, carrier gas is nitrogen, flow velocity 3ml/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310585508.8A CN104655739A (en) | 2013-11-21 | 2013-11-21 | Method of measuring the content of propanol in tail gas from fermentation of erythromycin through headspace gas chromatography |
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| CN201310585508.8A CN104655739A (en) | 2013-11-21 | 2013-11-21 | Method of measuring the content of propanol in tail gas from fermentation of erythromycin through headspace gas chromatography |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230152287A1 (en) * | 2020-01-23 | 2023-05-18 | East China University Of Science And Technology | Gas-sensitive-gas-chromatographic electronic nose instrument and online analysis method of multiple state parameters of fermentation and malodorous pollutant processes |
Citations (3)
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|---|---|---|---|---|
| WO2012127213A1 (en) * | 2011-03-18 | 2012-09-27 | The University Of Birmingham | Biomarkers |
| CN102879579A (en) * | 2012-09-18 | 2013-01-16 | 中国烟草总公司郑州烟草研究院 | Preparation method of standard substance used for detecting residual quantity of alcohol in cigarette paper |
| CN102998380A (en) * | 2012-10-15 | 2013-03-27 | 上海谱尼测试技术有限公司 | Method for detecting 21 volatile organic compounds (VOC) in tobacco packing box |
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2013
- 2013-11-21 CN CN201310585508.8A patent/CN104655739A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012127213A1 (en) * | 2011-03-18 | 2012-09-27 | The University Of Birmingham | Biomarkers |
| CN102879579A (en) * | 2012-09-18 | 2013-01-16 | 中国烟草总公司郑州烟草研究院 | Preparation method of standard substance used for detecting residual quantity of alcohol in cigarette paper |
| CN102998380A (en) * | 2012-10-15 | 2013-03-27 | 上海谱尼测试技术有限公司 | Method for detecting 21 volatile organic compounds (VOC) in tobacco packing box |
Non-Patent Citations (4)
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| RAQUEL OTERO 等: "Static headspace gas chromatographic method for quantitative determination of residual solvents in pharmaceutical drug substances according to European Pharmacopoeia requirements", 《JOURNAL OF CHROMATOGRAPHY A》, vol. 1057, no. 12, 19 December 2004 (2004-12-19), pages 193 - 201 * |
| 傅应华: "毛细管气相色谱内标法测定硫酸软骨素中的乙醇残留量", 《中国生化药物杂志》, vol. 30, no. 1, 20 February 2009 (2009-02-20), pages 41 - 43 * |
| 木书林 等: "顶空气相色谱法测定双氢青蒿素哌喹片中乙醇残留含量", 《药学研究》, vol. 32, no. 9, 30 September 2013 (2013-09-30), pages 504 - 506 * |
| 赵佳丽 等: "顶空毛细管气相色谱法测定倍他米松磷酸钠原料药中3种有机溶剂残留量", 《中国药房》, vol. 21, no. 21, 30 June 2010 (2010-06-30), pages 1999 - 2000 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230152287A1 (en) * | 2020-01-23 | 2023-05-18 | East China University Of Science And Technology | Gas-sensitive-gas-chromatographic electronic nose instrument and online analysis method of multiple state parameters of fermentation and malodorous pollutant processes |
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Application publication date: 20150527 |