CN101334388A - Food niacin content analytical method - Google Patents
Food niacin content analytical method Download PDFInfo
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- CN101334388A CN101334388A CNA2007100429483A CN200710042948A CN101334388A CN 101334388 A CN101334388 A CN 101334388A CN A2007100429483 A CNA2007100429483 A CN A2007100429483A CN 200710042948 A CN200710042948 A CN 200710042948A CN 101334388 A CN101334388 A CN 101334388A
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Abstract
The invention relates to an analytical method of nicotinic acid content in food, which adopts a pressurized capillary electrochromatography for analysis and comprises the steps as follows: the food to be analyzed is used for preparing sample solution; the prepared sample solution is directly injected into the pressurized capillary electrochromatography for carrying out the analysis; and an obtained chromatographic peak figure is compared with a standard chromatographic peak figure of the nicotinic acid, and the normalization method is used for calculating the percentage content of the nicotinic acid in the sample, etc. The mobile phase used by the analytical method of the invention is relatively simple, the using amount of the sample is less, the peak capacity is great, the analytical process is stable, and the method has good precision and separating effect.
Description
Technical field
The present invention relates to a kind of quantitative analysis method of material, relate in particular to nicotinic acid analysis on Content method in a kind of food.
Background technology
Nicotinic acid is also referred to as Cobastab
3, it is one of 13 kinds of vitamins of needed by human.Molten in the water part omitted, easily molten in sodium bicarbonate and sodium hydroxide solution.The assay of nicotinic acid is one of necessary index in the food, conventional chemical method of inspection complexity, waste time and energy, though the efficient liquid-phase chromatography method of development in recent years has improved the analysis speed of nicotinic acid, but because the polarity of nicotinic acid is big, often need to add ion-pairing agent in the tradition efficient liquid-phase chromatography method and separate, when increasing analysis cost, also increased analysis time.
Summary of the invention
Purpose of the present invention is exactly in order to solve the problem that above-mentioned prior art exists, nicotinic acid analysis on Content method in a kind of new food to be provided.
In order to achieve the above object, the present invention has adopted following technical scheme: nicotinic acid analysis on Content method in a kind of food, adopt the analysis of pressurization capillary electric chromatogram instrument, and may further comprise the steps:
A, preparation nicotinic acid standard solution
Accurately weighing nicotinic acid 10mg places the volumetric flask of 100ml, is the phosphate buffered solution dissolving of 5mmol and is diluted to scale with concentration, as the nicotinic acid standard solution;
B, preparation sample solution
Food samples to be analyzed is dissolved with suitable manner, and gained solution is collected filtered fluid as sample solution with 0.22 μ m filtering with microporous membrane;
C, sample introduction analysis
The nicotinic acid standard solution and the sample solution that prepare are distinguished directly to the analysis of pressurization capillary electric chromatogram instrument sample introduction, obtained nicotinic acid standard colors spectrogram and sample chromatogram figure;
D, contrast gained nicotinic acid standard colors spectrogram and sample chromatogram figure, the chromatographic peak of nicotinic acid in the mark sample, the integral area of nicotinic acid chromatographic peak in the calculation sample calculates the percentage composition of nicotinic acid in this sample with normalization method.
The analysis condition of the sample introduction analysis described in the step c is:
Capillary chromatographic column: adopt the quartz capillary column of the C18 filling of particle diameter 5 μ m, internal diameter 150 μ m, column length 55cm, effective column length 25cm;
Moving phase: the acetonitrile by the 5mmol phosphate solution of 85 parts by volume and 15 parts by volume is formulated;
Detect wavelength: 254nm;
Flow velocity: 0.05ml/min;
Voltage :+10kY.
Pressurization capillary electric chromatogram (pCEC) technology is the ingenious combination of liquid chromatography and capillary electrophoresis technique.It is that chromatograph packing material is filled in the kapillary, or at kapillary inside surface bonding, coating stationary phase, with the expulsive force of electroosmotic flow as moving phase, a kind of efficient Micro-Column Separation technology that the difference of the difference of each component partition factor between stationary phase and moving phase and migration rate in electric field per sample and realizing is separated has the double dominant of liquid chromatography and electrophoresis.The problem that it has solved the CE poor selectivity on the one hand, has been difficult to separate neutral substance has improved the separation efficiency of liquid chromatography on the other hand greatly.Compare with the analytical approach of prior art, adopt the pressurization capillary electric chromatogram method to analyze the content of nicotinic acid in the food, not only moving phase is simple relatively, and amount of samples is few, and peak capacity is big, and analytic process is stable, and method precision is good, and has good separating effect.
Description of drawings
Fig. 1 is the nicotinic acid standard colors spectrogram that adopts analytical approach of the present invention to obtain;
Fig. 2 is the chromatogram that the percentage composition of nicotinic acid in the employing analytical milk powder of the present invention obtains.
Embodiment
1, the preparation of nicotinic acid standard solution
Accurately weighing nicotinic acid 10mg places the volumetric flask of 100ml, is the phosphate buffered solution dissolving of 5mmol and is diluted to scale that with concentration (concentration is 1.0 * 10 as the nicotinic acid standard solution
-4G/ml).
2, the preparation of sample solution
Accurately weighing milk powder (flying crane board) 1g is in a small beaker, use the hot water dissolving, shake up the back, be transferred in the volumetric flask of 100ml with 0.22 μ m filtering with microporous membrane, dissolve and be diluted to scale with the phosphate buffered solution (pH=7.0) of 5mmol, as sample solution.
3, the making of nicotinic acid standard colors spectrogram
Directly to the analysis of pressurization capillary electric chromatogram instrument sample introduction, sample size is 700nl with the nicotinic acid standard solution for preparing, and be 20min analysis time; Analysis condition is: capillary chromatographic column adopts the quartz capillary column of the C18 filling of particle diameter 5 μ m, internal diameter 150 μ m, column length 55cm, effective column length 25cm; Employing is by the 5mmol phosphate solution of 85 parts by volume and the formulated analysis such as moving phase degree of grade of acetonitrile of 15 parts by volume; Detect wavelength: 254nm; Flow velocity: 0.05ml/min; Voltage :+10kV.Obtain nicotinic acid standard colors spectrogram as shown in Figure 1, wherein the peak located is that (concentration is 1.0 * 10 to nicotinic acid the time 9.746 '
-4G/ml) chromatographic peak.
4, nicotinic acid analysis on Content in the milk powder
Directly to the analysis of pressurization capillary electric chromatogram instrument sample introduction, sample size is 700nl with the sample solution for preparing, and be 20min analysis time; Analysis condition is: capillary chromatographic column adopts the quartz capillary column of the C18 filling of particle diameter 5 μ m, internal diameter 150 μ m, column length 55cm, effective column length 25c m; Employing is by the 5mmol phosphate solution of 85 parts by volume and the formulated analysis such as moving phase degree of grade of acetonitrile of 15 parts by volume; Detect wavelength: 254nm; Flow velocity: 0.05ml/min; Voltage :+10kV.Obtain chromatographic peak figure as shown in Figure 2, wherein the peak located is the chromatographic peak of nicotinic acid the time 9.820 '.
5, the calculating of the percentage composition of nicotinic acid in the sample
Contrast gained nicotinic acid standard colors spectrogram and sample chromatogram figure, the chromatographic peak of nicotinic acid in the mark sample, the integral area of nicotinic acid chromatographic peak in the calculation sample calculates the percentage composition of nicotinic acid in this sample with normalization method.
Method of the present invention adopts the pressurization capillary electric chromatogram instrument that the nicotinic acid content in the food is analyzed, in 20min, realized separating of nicotinic acid and other water soluble vitamins in the sample, experimental result shows, use pressurization capillary electric chromatogram (pCEC) analytical approach effectively to detect to the nicotinic acid content in the food, quantitatively accurately, cost is little.
Claims (2)
1, nicotinic acid analysis on Content method in a kind of food is characterized in that, adopts the analysis of pressurization capillary electric chromatogram instrument, may further comprise the steps:
A, preparation nicotinic acid standard solution
Accurately weighing nicotinic acid 10mg places the volumetric flask of 100ml, is the phosphate buffered solution dissolving of 5mmol and is diluted to scale with concentration, as the nicotinic acid standard solution;
B, preparation sample solution
Food samples to be analyzed is dissolved with suitable manner, and gained solution is collected filtered fluid as sample solution with 0.22 μ m filtering with microporous membrane;
C, sample introduction analysis
The nicotinic acid standard solution and the sample solution that prepare are distinguished directly to the analysis of pressurization capillary electric chromatogram instrument sample introduction, obtained nicotinic acid standard colors spectrogram and sample chromatogram figure;
D, contrast gained nicotinic acid standard colors spectrogram and sample chromatogram figure, the chromatographic peak of nicotinic acid in the mark sample, the integral area of nicotinic acid chromatographic peak in the calculation sample calculates the percentage composition of nicotinic acid in this sample with normalization method.
2, nicotinic acid analysis on Content method in the food according to claim 1, it is characterized in that: the analysis condition of the sample introduction analysis described in the step c is:
Capillary chromatographic column: adopt the quartz capillary column of the C18 filling of particle diameter 5 μ m, internal diameter 150 μ m, column length 55cm, effective column length 25cm;
Moving phase: the acetonitrile by the 5mmol phosphate solution of 85 parts by volume and 15 parts by volume is formulated;
Detect wavelength: 254nm;
Flow velocity: 0.05ml/min;
Voltage :+10kV.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100429483A CN101334388A (en) | 2007-06-28 | 2007-06-28 | Food niacin content analytical method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100429483A CN101334388A (en) | 2007-06-28 | 2007-06-28 | Food niacin content analytical method |
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|---|---|
| CN101334388A true CN101334388A (en) | 2008-12-31 |
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ID=40197123
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| CNA2007100429483A Pending CN101334388A (en) | 2007-06-28 | 2007-06-28 | Food niacin content analytical method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102980967A (en) * | 2012-12-28 | 2013-03-20 | 新希望乳业控股有限公司 | Method for detecting water soluble vitamins |
| CN105699465A (en) * | 2016-03-09 | 2016-06-22 | 福州大学 | Method for continuously separating synthetic pigments in multiple modes with pCEC (pressurized capillary electrochromatography) |
| CN111272912A (en) * | 2020-03-20 | 2020-06-12 | 山东省食品药品检验研究院 | Method for measuring nicotinic acid and nicotinamide in infant rice flour by solid-phase extraction-high performance liquid chromatography |
-
2007
- 2007-06-28 CN CNA2007100429483A patent/CN101334388A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102980967A (en) * | 2012-12-28 | 2013-03-20 | 新希望乳业控股有限公司 | Method for detecting water soluble vitamins |
| CN105699465A (en) * | 2016-03-09 | 2016-06-22 | 福州大学 | Method for continuously separating synthetic pigments in multiple modes with pCEC (pressurized capillary electrochromatography) |
| CN105699465B (en) * | 2016-03-09 | 2018-08-17 | 福州大学 | A kind of method that pressurization capillary electric chromatogram multi-mode continuously detaches synthetic dyestuff |
| CN111272912A (en) * | 2020-03-20 | 2020-06-12 | 山东省食品药品检验研究院 | Method for measuring nicotinic acid and nicotinamide in infant rice flour by solid-phase extraction-high performance liquid chromatography |
| CN111272912B (en) * | 2020-03-20 | 2022-02-01 | 山东省食品药品检验研究院 | Method for measuring nicotinic acid and nicotinamide in infant rice flour by solid-phase extraction-high performance liquid chromatography |
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Open date: 20081231 |