CN104807916A - Method for detecting rongalit in food by gas chromatograph mass spectrometer - Google Patents
Method for detecting rongalit in food by gas chromatograph mass spectrometer Download PDFInfo
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- CN104807916A CN104807916A CN201510242691.0A CN201510242691A CN104807916A CN 104807916 A CN104807916 A CN 104807916A CN 201510242691 A CN201510242691 A CN 201510242691A CN 104807916 A CN104807916 A CN 104807916A
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Abstract
The invention discloses a method for detecting rongalit in food by a gas chromatograph mass spectrometer. The method comprises the following steps that 1, 1g of food specimens are added into a top hollow bottle; 1 to 3ml pf 0.05 mol/L EDTA (ethylene diamine tetraacetic acid) solution and 1 to 3 ml of 0.05 mol/L sodium acetate solution are added, and the materials are compacted after being uniformly stirred and are fed onto a machine to be tested; 2, the gas chromatograph mass spectrometer is adopted for testing the content of sodium formaldehyde sulfoxylate in the top hollow bottle. The invention aims at providing the method for detecting the rongalit in food by the gas chromatograph mass spectrometer with the advantages that the testing is accurate, the operation is simple, and the time consumption is low.
Description
Technical field
The present invention relates to detection field, particularly a kind of Gas-phase acidity instrument detects the method for the sodium formaldehyde sulfoxylate in food.
Background technology
GB/T 21126-2007 and DB34/T 1108-2009 have recorded the method by sodium formaldehyde sulfoxylate in liquid chromatographic detection food, but the method that have employed extraction carries out sample pretreatment, but the method processing time is long, and the extracting substances for trace exists error.
Summary of the invention
The object of the present invention is to provide a kind of method of the sodium formaldehyde sulfoxylate measured in accurate, simple to operate, that the used time is short Gas-phase acidity instrument detection food.
Technical scheme of the present invention is: a kind of Gas-phase acidity instrument detects the method for the sodium formaldehyde sulfoxylate in food, comprises the following steps:
Step 1: add 1g food sample in ml headspace bottle, add the EDTA solution of 1 ~ 3ml0.05mol/L, the sodium acetate solution of 1 ~ 3ml0.05mol/L, after stirring, in compacting, machine is to be measured;
Step 2: adopt gas-mass spectrometer to measure the content of rongalite in ml headspace bottle, wherein, the setting parameter of gas-mass spectrometer is as follows:
Chromatographic column: Phenomenex 60m × 0.50mm, 3.2 μm;
The column temperature program of chromatographic column: initial temperature 40 DEG C, rises to 110 DEG C with 10 DEG C/min after keeping 5min, keeps 5min;
Injector temperature: 300 DEG C; Interface temperature: 280 DEG C; Quadrupole rod temperature: 150 DEG C; Ion source temperature: 230 DEG C;
Carrier gas: the helium of purity >=99.999%, current constant mode, flow velocity 0.4mL/min;
Ionization mode: EI; Ionizing energy: 70ev;
Monitoring mode: full scan/Salbutamol Selected Ion Monitoring is drainage pattern simultaneously; Monitor ion range: 20 ~ 130m/z;
Input mode: solvent vent mode, sample size: 5.0 μ L;
Solvent delay 1min.
Beneficial effect of the present invention is as follows:
Pre-treatment simple and fast of the present invention, solvent is used to greatly reduce that (national standard method solvent load is 60ml, solvent load of the present invention is 5ml), experimental period shortens greatly, and (national standard method needs to extract 40min consuming time, water-bath 40min consuming time, extract 1.5h consuming time, the present invention only need spend 5min), this method detection sensitivity is higher, and concentrations is 1 μ g/kg.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1
Step 1: add 1g food sample in ml headspace bottle, add the EDTA solution of 2ml0.05mol/L, the sodium acetate solution of 2ml0.05mol/L, after stirring, in compacting, machine is to be measured;
Step 2: adopt gas-mass spectrometer to measure the content of rongalite in ml headspace bottle, wherein, the setting parameter of gas-mass spectrometer is as follows:
Chromatographic column: Phenomenex 60m × 0.50mm, 3.2 μm;
The column temperature program of chromatographic column: initial temperature 40 DEG C, rises to 110 DEG C with 10 DEG C/min after keeping 5min, keeps 5min;
Injector temperature: 300 DEG C; Interface temperature: 280 DEG C; Quadrupole rod temperature: 150 DEG C; Ion source temperature: 230 DEG C;
Carrier gas: the helium of purity >=99.999%, current constant mode, flow velocity 0.4mL/min;
Ionization mode: EI; Ionizing energy: 70ev;
Monitoring mode: full scan/Salbutamol Selected Ion Monitoring is drainage pattern simultaneously; Monitor ion range (m/z): 20 ~ 130;
Input mode: solvent vent mode, sample size: 5.0 μ L;
Solvent delay 1min.
Embodiment 2
Step 1: add 1g food sample in ml headspace bottle, add the EDTA solution of 1ml0.05mol/L, the sodium acetate solution of 3ml0.05mol/L, after stirring, in compacting, machine is to be measured;
Step 2: adopt gas-mass spectrometer to measure the content of rongalite in ml headspace bottle, wherein, the setting parameter of gas-mass spectrometer is as follows:
Chromatographic column: Phenomenex 60m × 0.50mm, 3.2 μm;
The column temperature program of chromatographic column: initial temperature 40 DEG C, rises to 110 DEG C with 10 DEG C/min after keeping 5min, keeps 5min;
Injector temperature: 300 DEG C; Interface temperature: 280 DEG C; Quadrupole rod temperature: 150 DEG C; Ion source temperature: 230 DEG C;
Carrier gas: the helium of purity >=99.999%, current constant mode, flow velocity 0.4mL/min;
Ionization mode: EI; Ionizing energy: 70ev;
Monitoring mode: full scan/Salbutamol Selected Ion Monitoring is drainage pattern simultaneously; Monitor ion range (m/z): 20 ~ 130;
Input mode: solvent vent mode, sample size: 5.0 μ L;
Solvent delay 1min.
Above-described embodiment 1 and 2 pre-treatment simple and fast, solvent is used to greatly reduce that (national standard method solvent load is 60ml, solvent load of the present invention is 5ml), experimental period shortens greatly, and (national standard method needs to extract 40min consuming time, water-bath 40min consuming time, extract 1.5h consuming time, the present invention only need spend 5min), this method detection sensitivity is higher, and concentrations is 1 μ g/kg.
Above-describedly be only preferred embodiment of the present invention, all do within the scope of the spirit and principles in the present invention any amendment, equivalently to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. Gas-phase acidity instrument detects a method for the sodium formaldehyde sulfoxylate in food, it is characterized in that, comprises the following steps:
Step 1: add 1g food sample in ml headspace bottle, add the EDTA solution of 1 ~ 3ml0.05mol/L, the sodium acetate solution of 1 ~ 3ml0.05mol/L, after stirring, in compacting, machine is to be measured;
Step 2: adopt gas-mass spectrometer to measure the content of rongalite in ml headspace bottle, wherein, the setting parameter of gas-mass spectrometer is as follows:
Chromatographic column: Phenomenex 60m × 0.50mm, 3.2 μm;
The column temperature program of chromatographic column: initial temperature 40 DEG C, rises to 110 DEG C with 10 DEG C/min after keeping 5min, keeps 5min;
Injector temperature: 300 DEG C; Interface temperature: 280 DEG C; Quadrupole rod temperature: 150 DEG C; Ion source temperature: 230 DEG C;
Carrier gas: the helium of purity >=99.999%, current constant mode, flow velocity 0.4mL/min;
Ionization mode: EI; Ionizing energy: 70ev;
Monitoring mode: full scan/Salbutamol Selected Ion Monitoring is drainage pattern simultaneously; Monitor ion range: 20 ~ 130m/z;
Input mode: solvent vent mode, sample size: 5.0 μ L;
Solvent delay 1min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510242691.0A CN104807916A (en) | 2015-05-12 | 2015-05-12 | Method for detecting rongalit in food by gas chromatograph mass spectrometer |
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| CN201510242691.0A CN104807916A (en) | 2015-05-12 | 2015-05-12 | Method for detecting rongalit in food by gas chromatograph mass spectrometer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107817288A (en) * | 2017-09-04 | 2018-03-20 | 浙江工商大学 | The electrochemical determination method of sodium formaldehyde sulfoxylate content when CTAB CNT Chit modified electrodes and sulphite coexist |
| CN108169372A (en) * | 2017-12-22 | 2018-06-15 | 上海微谱化工技术服务有限公司 | The assay method of electroplating wastewater complexing agent |
| CN108362747A (en) * | 2017-12-30 | 2018-08-03 | 常州市奥普泰科光电有限公司 | A kind of preparation method and its application method of detection sodium formaldehyde sulfoxylate electrochemical sensor |
-
2015
- 2015-05-12 CN CN201510242691.0A patent/CN104807916A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107817288A (en) * | 2017-09-04 | 2018-03-20 | 浙江工商大学 | The electrochemical determination method of sodium formaldehyde sulfoxylate content when CTAB CNT Chit modified electrodes and sulphite coexist |
| CN107817288B (en) * | 2017-09-04 | 2019-12-03 | 浙江工商大学 | The electrochemical determination method of sodium formaldehyde sulfoxylate content when CTAB-CNT-Chit modified electrode and sulphite coexist |
| CN108169372A (en) * | 2017-12-22 | 2018-06-15 | 上海微谱化工技术服务有限公司 | The assay method of electroplating wastewater complexing agent |
| CN108169372B (en) * | 2017-12-22 | 2020-11-10 | 上海微谱化工技术服务有限公司 | Method for measuring complexing agent in electroplating wastewater |
| CN108362747A (en) * | 2017-12-30 | 2018-08-03 | 常州市奥普泰科光电有限公司 | A kind of preparation method and its application method of detection sodium formaldehyde sulfoxylate electrochemical sensor |
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Application publication date: 20150729 |