CN105866308A - Method of utilizing gas chromatography to detect cyclamate - Google Patents
Method of utilizing gas chromatography to detect cyclamate Download PDFInfo
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- CN105866308A CN105866308A CN201610303596.1A CN201610303596A CN105866308A CN 105866308 A CN105866308 A CN 105866308A CN 201610303596 A CN201610303596 A CN 201610303596A CN 105866308 A CN105866308 A CN 105866308A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention discloses a method of utilizing gas chromatography to detect cyclamate. The method includes: 1), using alkaline liquid to adjust pH of a sample to be alkaline, and treating the sample through ice bath; 2), mixing a sulfuric acid solution with the sample after going through ice bath at 25-35 DEG C, adding a sodium nitrite solution for second mixing under the condition of ice bath, adding normal hexane, shaking, layering, and taking supernatant; 3), detecting the supernatant through a gas chromatograph, wherein split ratio os 1:48-1:51, temperature of a chromatographic column, and temperature of a sample inlet is 175-185 DEG C. The method has the advantages of simple operation, high recovery rate, high precision and high sensitivity.
Description
Technical field
The present invention relates to the detection method of honey element, in particular it relates to one utilizes gas chromatographic detection to eat
The method of honey element in product.
Background technology
Honey element, its chemical name is sodium cyclohexylsulfamate, is additive conventional in food production
.Honey element is a kind of conventional sweetener, and its sugariness is 30-40 times of sucrose, but the consumption of honey element
Need in suitable dosage, if the beverage of the most edible honey element content overproof or other food, will
Because liver and the nervous system of human body are worked the mischief by excess intake, particularly to the ability of metabolism relatively
Weak old man, pregnant woman, child's harm become apparent from；Therefore, the detection of honey element field of food to close weight
Want.
At present, measurement of Sodium Cyclamate in Food method generally uses GB GB/T 5009.97-2003 " food
The mensuration of sodium cyclohexylsulfamate in product " gas chromatography, the principle of the method is: at sulfuric acid medium
Middle honey element and natrium nitrosum react generation cyclohexanol nitrites, utilize gas chromatography carry out qualitative and
Quantitatively；Concretely comprise the following steps: adding 5mL concentration in the coupon prepared is that 50g/L natrium nitrosum is molten
Liquid, 5mL concentration is 100g/L sulfuric acid solution, shakes up, and places 30min, and often shake in ice bath
Dynamic, the most accurately add 10mL n-hexane, 5g sodium chloride, shake up and vibrate on rearmounted eddy mixer
1min, after stratification, the centrifugation of sucking-off hexane layer, to be measured.Although the method is able to detect that food
The content of the honey element in product, but still suffer from certain defect, and the pre-treatment such as sample is loaded down with trivial details, derivative
In course of reaction, reaction mechanism is complicated, and accessory substance is various.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing gas chromatographic detection Determination of Saccharin in Food, the party
Method has feature simple to operate, that the rate of recovery is high, precision is high and highly sensitive.
To achieve these goals, the invention provides one and utilize gas chromatographic detection Determination of Saccharin in Food
Method, the method includes:
1) by alkali lye, the pH of sample is adjusted to alkalescence, then carries out ice bath process；
2) sample after sulfuric acid solution and ice bath is carried out the first mixed processing at 25-35 DEG C, then add
Enter sodium nitrite solution under condition of ice bath, carry out the second mixing, be layered also after being subsequently adding n-hexane concussion
Take upper liquid；
3) upper liquid is detected by gas chromatograph；
Wherein, split ratio is 1:48-1:51, temperature 75-85 DEG C of chromatographic column, and the temperature of injection port is
175-185℃。
Preferably, in step 3) in, post flow is 1.6-1.8mL/min.
Preferably, in step 3) in, in a detector, the flow velocity of hydrogen is 34-38mL/min, empty
The flow velocity of gas is 315-325mL/min.
Preferably, in step 3) in, sample size is 0.8-1.2 μ L.
Preferably, in step 2) in, the concentration of sulfuric acid solution is 90-120g/L, sodium nitrite solution
Concentration is 45-55g/L.
Preferably, in the case of sample is fluid sample, relative to 20g sample, the use of sulfuric acid solution
Amount is 4-6mL, and the consumption of sodium nitrite solution is 4-6mL, and the consumption of n-hexane is 8-12mL；
Or, in the case of sample is solid sample, relative to 0.4g sample, the consumption of sulfuric acid solution
For 4-6mL, the consumption of sodium nitrite solution is 4-6mL, and the consumption of n-hexane is 8-12mL.
Preferably, the first mixing at least meets following condition: mixing temperature is 25-35 DEG C, incorporation time
For 8-12min；The time of the second mixing is 25-35min；
Preferably, in the case of sample is solid sample, in step 2) before, method also includes:
Grind after sample is mixed with abrasive sand, be then dissolved in water, filter formation sample solution.
Preferably, relative to 2g sample, the consumption of water is 97-99mL.
Preferably, abrasive sand is chromatographic silica gel and/or sea sand.
Preferably, in step 3) in, chromatograph is the gas phase look of Japan Shimadzu Corporation trade mark GC-2010
Spectrometer；Capillary column is the capillary of Agilent company trade mark J&W GC Columns CP-Wax 57CB
Tubing string.
Preferably, the size of capillary column is 50m × 0.25mm × 0.2um.
By technique scheme, the present invention is by GB GB/T 5009.97-2003 in prior art
In detection method improve, during by adjusting reaction temperature, reagent dosage, extraction time and reaction
Between and improve chromatographic condition, reduce the Interference Peaks in solvent, reduce the generation of accessory substance, hence it is evident that improve
Precision and reappearance, it is thus achieved that the most linear and detection limit, improve sensitivity simultaneously.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that this place is retouched
The detailed description of the invention stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of method utilizing gas chromatographic detection Determination of Saccharin in Food, the method bag
Include:
1) by alkali lye, the pH of sample is adjusted to alkalescence, then carries out ice bath process；
2) sample after sulfuric acid solution and ice bath is carried out the first mixed processing at 25-35 DEG C, then add
Enter sodium nitrite solution under condition of ice bath, carry out the second mixing, be layered also after being subsequently adding n-hexane concussion
Take upper liquid；
3) upper liquid is detected by gas chromatograph；
Wherein, split ratio is 1:48-1:51, temperature 75-85 DEG C of chromatographic column, and the temperature of injection port is
175-185℃。
In above-mentioned detection method, post flow can select in wide scope, but so that should
Method has that the more excellent rate of recovery is high, precision is high and highly sensitive, it is preferable that in step 3) in,
Post flow is 1.6-1.8mL/min.
Step 3 in the present invention) in, in detector, gas flow can select in wide scope, but
It is that the more excellent rate of recovery is high, precision is high and highly sensitive so that the method has, it is preferable that
In a detector, the flow velocity of hydrogen is 34-38mL/min, and the flow velocity of air is 315-325mL/min.
Step 3 in the present invention) in, sample size can select in wide scope, but so that
The method has that the more excellent rate of recovery is high, precision is high and highly sensitive, it is preferable that in step 3)
In, sample size is 0.8-1.2 μ L.
Step 2 in the present invention) in, the concentration of each material can select in wide scope, but is
The method is had, and the more excellent rate of recovery is high, precision is high and highly sensitive, it is preferable that in step
Rapid 2) in, the concentration of sulfuric acid solution is 90-120g/L, and the concentration of sodium nitrite solution is 45-55g/L.
Step 2 in the present invention) in, the consumption of each material can select in wide scope, but is
The method is had, and the more excellent rate of recovery is high, precision is high and highly sensitive, it is preferable that at sample
In the case of product are fluid sample, relative to 20g sample, the consumption of sulfuric acid solution is 4-6mL, nitrous
The consumption of acid sodium solution is 4-6mL, and the consumption of n-hexane is 8-12mL；Or, it is solid at sample
In the case of sample, relative to 0.4g sample, the consumption of sulfuric acid solution is 4-6mL, sodium nitrite solution
Consumption be 4-6mL, the consumption of n-hexane is 8-12mL.
Step 2 in the present invention) in, mixing condition can select in wide scope, but in order to make
The method has that the more excellent rate of recovery is high, precision is high and highly sensitive, it is preferable that the first mixing
At least meeting following condition: mixing temperature is 25-35 DEG C, incorporation time is 8-12min；Second mixing
Time is 25-35min.
In the present invention, so that the method has, the more excellent rate of recovery is high, precision is high and sensitive
Degree height, it is preferable that in the case of sample is solid sample, in step 2) before, method also includes:
Grind after sample is mixed with abrasive sand, be then dissolved in water, filter formation sample solution.Wherein, water
Consumption can select in wide scope, so that the rate of recovery is high, precision is high and sensitivity high energy
Improve further, it is preferable that relative to 2g sample, the consumption of water is 97-99mL.The kind of abrasive sand
Class can also select in wide scope, but the rate of recovery is high, precision is high and clever in order to improve further
Sensitivity, it is preferable that abrasive sand is chromatographic silica gel and/or sea sand.
Step 3 in the present invention) in, the concrete kind of chromatograph and capillary column can be at wide model
Enclose interior selection, it is preferable that in step 3) in, chromatograph is Japan Shimadzu Corporation trade mark GC-2010
Gas chromatograph；Capillary column is Agilent company trade mark J&W GC Columns CP-Wax 57CB
Capillary column, it is highly preferred that the size of capillary column is 50m × 0.25mm × 0.2um.
Hereinafter will be described the present invention by embodiment.
Embodiment 1
1) by alkali lye, the pH of white wine is adjusted to alkalescence, then carries out ice bath process and form sample solution；
2) 20g sample solution is mixed at 30 DEG C with the sulfuric acid solution 5mL that concentration is 100g/L
Close 10min, be subsequently added into the sodium nitrite solution 5mL that concentration is 50g/L and react 30min, then add
It is layered after entering the concussion of 10mL n-hexane whirlpool and takes upper liquid；
3) 1 μ L upper liquid is examined by the gas chromatograph of Japan Shimadzu Corporation trade mark GC-2010
Survey；
Wherein, chromatographic condition is: capillary column is Agilent company trade mark J&W GC Columns
The capillary column of CP-Wax 57CB, the size of capillary column is 50m × 0.25mm × 0.2um；Shunting
Ratio is 1:50, the temperature of chromatographic column 80 DEG C, and the temperature of injection port is 180 DEG C, and post flow is
1.78mL/min；In a detector, the flow velocity of hydrogen is 36mL/min, and the flow velocity of air is
320mL/min。
Embodiment 2
1) by alkali lye, the pH of white wine is adjusted to alkalescence, then carries out ice bath process and form sample solution；
2) 20g sample solution is mixed at 25 DEG C with the sulfuric acid solution 4mL that concentration is 9g/L
8min, is subsequently added into the sodium nitrite solution 4mL that concentration is 45g/L and reacts 25min, be subsequently adding
It is layered after the concussion of 8mL n-hexane whirlpool and takes upper liquid；
3) 0.8 μ L upper liquid is carried out by the gas chromatograph of Japan Shimadzu Corporation trade mark GC-2010
Detection；
Wherein, chromatographic condition is: capillary column is Agilent company trade mark J&W GC Columns
The capillary column of CP-Wax 57CB, the size of capillary column is 50m × 0.25mm × 0.2um；Shunting
Ratio is 1:48, the temperature of chromatographic column 75 DEG C, and the temperature of injection port is 175 DEG C, and post flow is 1.6mL/min；
In a detector, the flow velocity of hydrogen is 34mL/min, and the flow velocity of air is 315mL/min.
Embodiment 3
1) by alkali lye, the pH of white wine is adjusted to alkalescence, then carries out ice bath process and form sample solution；
2) 20g sample solution is mixed at 35 DEG C with the sulfuric acid solution 6mL that concentration is 120g/L
Close 12min, be subsequently added into the sodium nitrite solution 6mL that concentration is 55g/L and react 35min, then add
It is layered after entering the concussion of 12mL n-hexane whirlpool and takes upper liquid；
3) 1.2 μ L upper liquid are carried out by the gas chromatograph of Japan Shimadzu Corporation trade mark GC-2010
Detection；
Wherein, chromatographic condition is: capillary column is Agilent company trade mark J&W GC Columns
The capillary column of CP-Wax 57CB, the size of capillary column is 50m × 0.25mm × 0.2um；Shunting
Ratio is 1:51, the temperature of chromatographic column 85 DEG C, and the temperature of injection port is 185 DEG C, and post flow is 1.8mL/min；
In a detector, the flow velocity of hydrogen is 38mL/min, and the flow velocity of air is 325mL/min.
In detection example 1-3, result is: the content of honey element is 0mg/kg, and the rate of recovery is 98-95%.
Comparative example 1
" mensuration of Cyclamate in Foods " according to GB GB/T 5009.97-2003 regulation
Detecting the honey element in above-mentioned white wine, result is: the content of honey element is 0mg/kg, reclaims
Rate is 97.4%.
By above-described embodiment and comparative example, the detection method that the present invention provides has more excellent returning
Yield.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
Execute the detail in mode, in the technology concept of the present invention, can be to the technical side of the present invention
Case carries out multiple simple variant, and these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technology described in above-mentioned detailed description of the invention is special
Levy, in the case of reconcilable, can be combined by any suitable means, in order to avoid need not
The repetition wanted, various possible combinations are illustrated by the present invention the most separately.
Additionally, can also be combined between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the method utilizing gas chromatographic detection Determination of Saccharin in Food, it is characterised in that described side
Method includes:
1) by alkali lye, the pH of sample is adjusted to alkalescence, then carries out ice bath process；
2) the described sample after sulfuric acid solution and ice bath is carried out the first mixed processing at 25-35 DEG C, connect
Addition sodium nitrite solution under condition of ice bath, carry out the second mixing, divide after being subsequently adding n-hexane concussion
Layer also takes upper liquid；
3) described upper liquid is detected by gas chromatograph；
Wherein, split ratio is 1:48-1:51, temperature 75-85 DEG C of chromatographic column, and the temperature of injection port is
175-185℃。
Method the most according to claim 1, wherein, in step 3) in, post flow is
1.6-1.8mL/min。
Method the most according to claim 2, wherein, in step 3) in, in a detector, hydrogen
The flow velocity of gas is 34-38mL/min, and the flow velocity of air is 315-325mL/min.
Method the most according to claim 2, wherein, in step 3) in, sample size is 0.8-1.2 μ L.
5. according to the method described in any one in claim 1-4, wherein, in step 2) in, institute
The concentration stating sulfuric acid solution is 90-120g/L, and the concentration of described sodium nitrite solution is 45-55g/L.
Method the most according to claim 5, wherein, is the situation of fluid sample at described sample
Under, relative to sample described in 20g, the consumption of described sulfuric acid solution is 4-6mL, and described natrium nitrosum is molten
The consumption of liquid is 4-6mL, and the consumption of described n-hexane is 8-12mL；
Or, in the case of described sample is solid sample, relative to sample described in 0.4g, described sulphur
The consumption of acid solution is 4-6mL, and the consumption of described sodium nitrite solution is 4-6mL, described n-hexane
Consumption is 8-12mL.
Method the most according to claim 6, wherein, described first mixing at least meets following bar
Part: mixing temperature is 25-35 DEG C, incorporation time is 8-12min；Described second mixing time be
25-35min。
8. it is according to the method described in claim 5 or 6, wherein, solid sample at described sample
In the case of, in step 2) before, described method also includes: grind after being mixed with abrasive sand by described sample
Mill, is then dissolved in water, filters formation sample solution.
Method the most according to claim 8, wherein, relative to sample described in 2g, described water
Consumption is 97-99mL；
Preferably, described abrasive sand is chromatographic silica gel and/or sea sand.
10. according to the method described in any one in claim 1-4, wherein, in step 3) in,
Described gas chromatograph is the gas chromatograph of Japan Shimadzu Corporation trade mark GC-2010；Capillary column is
The capillary column of Agilent company trade mark J&W GC Columns CP-Wax 57CB；
Preferably, the size of described capillary column is 50m × 0.25mm × 0.2um.
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Citations (4)
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| WO2008157228A1 (en) * | 2007-06-13 | 2008-12-24 | Cambrex Charles City, Inc. | New methods for taste-masking |
| CN101799461A (en) * | 2010-04-27 | 2010-08-11 | 中国烟草总公司郑州烟草研究院 | Method for testing sodium N-cyclohexylsulfamate content in tobacco additives |
| CN103257200A (en) * | 2012-02-17 | 2013-08-21 | 谱尼测试科技股份有限公司 | Method of determining content of sodium cyclamate in food through high performance liquid chromatography with ultraviolet detector |
| CN105259263A (en) * | 2015-10-16 | 2016-01-20 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for detecting content of sodium cyclamate in food |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008157228A1 (en) * | 2007-06-13 | 2008-12-24 | Cambrex Charles City, Inc. | New methods for taste-masking |
| CN101799461A (en) * | 2010-04-27 | 2010-08-11 | 中国烟草总公司郑州烟草研究院 | Method for testing sodium N-cyclohexylsulfamate content in tobacco additives |
| CN103257200A (en) * | 2012-02-17 | 2013-08-21 | 谱尼测试科技股份有限公司 | Method of determining content of sodium cyclamate in food through high performance liquid chromatography with ultraviolet detector |
| CN105259263A (en) * | 2015-10-16 | 2016-01-20 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for detecting content of sodium cyclamate in food |
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Application publication date: 20160817 |