CN105572237A - High performance liquid chromatographic method for rapid quantitative assessment of honey quality - Google Patents
High performance liquid chromatographic method for rapid quantitative assessment of honey quality Download PDFInfo
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- CN105572237A CN105572237A CN201410535926.0A CN201410535926A CN105572237A CN 105572237 A CN105572237 A CN 105572237A CN 201410535926 A CN201410535926 A CN 201410535926A CN 105572237 A CN105572237 A CN 105572237A
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Abstract
The invention discloses a high performance liquid chromatographic method for rapid quantitative assessment of honey quality. According to the method, 10 to 20 parts of a representative honey sample is collected, and a proper amount of the sample is weighed and pre-treated by using pure acetonitrile for high performance liquid chromatographic detection; a special analytical column for sugar is used as a chromatographic column, and acetonitrile-water (75: 25) is used as a mobile phase; a differential refraction detector is used for detection, an external standard method is used for quantification, and the contents of glucose, fructose and cane sugar are calculated. The method provided by the invention employs high performance liquid chromatography and the special analytical column for sugar to successively separate glucose, fructose and cane sugar in honey, acetonitrile-water (75: 25) is used as the mobile phase, and chromatographic separation is finished in about 15 min; the method has good separation effect, high determination repeatability, detection sensitivity and a recovery rate of 97.0 to 98.9% and is easy in pretreatment and operation; acetonitrile and water are used as solvents and acetonitrile and water can be recycled and are free of pollution, so clean production is realized; and the method protects the interests of consumers and is of guiding significance to production of honey production enterprises.
Description
Technical field
The present invention relates to a kind of chromatographic process of quantifying honey quality, particularly relate to a kind of efficient liquid-phase chromatography method of rapidly quantifying honey quality.
Background technology
Containing more than 180 kinds of active substances in honey, its principal ingredient is the FOS of fructose and glucose and 4% ~ 5%, in addition in honey also containing abundant amino acid, vitamin, organized enzyme, flavonoids, Polyphenols, carotenoid isoreactivity material and several mineral materials.Honey has the multiple physiologically actives such as anti-oxidant, antibacterial, acceleration of wound reparation, develop immunitypty, thus honey is not only originated by as the direct effective nutritional supplementation of one, and is applied to treatment hepatitis, cancer, wound infection, constipation and improves gastrointestinal function, raising immunity of organisms etc.
In recent years, honey, as a kind of natural health-care products of medicine-food two-purpose, is subject to increasing favor.China is bee-keeping and honey big export country, and the nineties in 20th century, China's honey export volume accounted for 40% of world's year volume of trade.But honey is one very easily adulteration of food, in recent years due to the quality problems such as adulterated, make the prestige of China's honey product more and more lower, export volume declines year by year.In order to specification honey market, the national standardization council has issued GB18796-2005 " honey " state compulsory standard on October 26th, 2005, and regulation enforcement from 1 day March in 2006.GB18796-2005 regulation Fructose in Honey and glucose content should be more than or equal to 60%, and the honey importer such as European Union, Japan also specify the parameter such as Reducing Sugar in Honey content and fruit Portugal ratio.Therefore, the assay method of a series of Reducing Sugar in Honey must be set up, both can Protection of consumer interests, to the production of honey manufacturing enterprise, there is directive significance again.
At present, titrimetry, polarimetry, thin-layer chromatography, high performance liquid chromatography, chromatography of ions pulsed amperometric method, gas chromatography mass spectrometry method, high performance capillary electrophoresis, nuclear magnetic resonance method etc. are mainly contained about Reducing Sugar in Honey method for measuring.But traditional titrimetry, thin-layered chromatography, Optical Rotation complex operation and accuracy are not high.High performance liquid chromatography adopts differential refraction detector or evaporative light-scattering detector, and sensitivity is lower, and affects greatly by temperature, mobile phase.Chromatography of ions pulsed amperometric method is used for the mensuration of monose, disaccharides, Small molecular oligosaccharides, have highly sensitive, selectivity good, need not derive, easy and simple to handle etc. a little.But chromatography of ions requires higher to reagent, sample introduction sample, and sample pre-treatments step requires strict, and needs special chromatography of ions and pulsed amperometry.The method apparatus expensive such as Capillary Electrophoresis, gas chromatography mass spectrometry, nuclear magnetic resonance, not easily universal in middle-size and small-size honey manufacturing enterprise at home.
Summary of the invention
The present invention adopts high performance liquid chromatography, is intended to set up the method for the fructose in a kind of Simultaneously test honey, glucose, sucrose.
For achieving the above object, an efficient liquid-phase chromatography method for rapidly quantifying honey quality, present invention employs following technical scheme: collect representative honey sample 10 ~ 20 parts, take appropriate amount of sample, with pure acetonitrile pre-treatment, detect for high performance liquid chromatography.With sugared dedicated analysis post for chromatographic column, acetonitrile-water (75: 25) is mobile phase.Detect with differential refraction detector, quantified by external standard method, calculate the content of glucose, fructose and sucrose.
Described chromatographic column is sugared dedicated analysis post (4mm × 250mm).
Described chromatographic column column temperature is 35 DEG C.
Described mobile phase flow rate is 1ml/min.
Described mobile phase sample size is 10 μ L.
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is:
Be separated, measure the research report of the soluble sugar in honey seldom with high performance liquid chromatography, the present invention utilizes high performance liquid chromatography to be successfully separated fructose, glucose, sucrose in honey with sugared dedicated analysis post, with acetonitrile: water=75:25 is mobile phase, namely about 15min completes chromatographic separation process, good separation, the repeatability of mensuration is high, detects sensitive, the recovery between 97.0% ~ 98.9%, pre-treatment and simple to operate.Solvent of the present invention adopts acetonitrile and water, and recoverable is pollution-free, realizes cleaner production.Both Protection of consumer interests, have directive significance to the production of honey manufacturing enterprise again.
Embodiment
The efficient liquid-phase chromatography method of embodiment 1 one kinds of rapidly quantifying honey qualities
1, sample preparation
Take fructose, glucose respectively about 100mg, sucrose be about 20mg, accurately weighed, put in 50ml measuring bottle, dissolve with mobile phase and be diluted to scale, shaking up.
Take 0.5g honey sample, add the pure acetonitrile of 2mL, 65 DEG C of water-bath 10min, the centrifugal 20min of 10000r/min, Aspirate supernatant is in the volumetric flask of 25mL, and residue adds 3mL distilled water, 65 DEG C of water-bath 10min, 10000r/min is centrifugal, merges supernatant, according to said method extracts once again, merge supernatant, and be settled to 25mL with distilled water, extract 5mL organic system (0.45 μm of filter membrane) and filter, detect for high performance liquid chromatography.
2, chromatographiccondition
Shimadzu LC-20A liquid chromatograph, chromatographic column is sugared dedicated analysis post (4mm × 250mm).Differential refraction detector.Mobile phase: acetonitrile-water (75: 25), column temperature 35 DEG C, flow 1ml/min, sample size 10 μ L.
3, the mensuration of typical curve
The standard working solution of accurate preparation 0.2mg/mL, 1.0mg/mL, 2.5mg/mL, 5.0mg/mL and 10.0mg/mL, carries out liquid-phase chromatographic analysis.Take concentration as X-axis, peak area is that Y-axis carries out linear regression, production standard curve.
4, set sampling amount is analyzed per sample, in having investigated every milliliter containing fructose, glucose be 0.4,0.6,0.8,1.0,1.2mg with every milliliter in contain sucrose 0.1,0.2,0.3,0.4, the linear relationship of 0.5mg, recurrence through concentration and peak area relation calculates, the regression equation of fructose is Y=45+382360X, coefficient R 2=0.999; The regression equation of glucose is Y=120+322658X, coefficient R 2=0.9991; The regression equation of sucrose is Y=75+78054X, coefficient R 2=0.9992.
The honey 10 batches of different cultivars and source with above-mentioned methods analyst, typical sample result sees the following form 1.Analytical data is bright: 1. the content range of the good natural honey fructose of quality, glucose is 30% ~ 35%, and cane sugar content is below 2%; The honey of 2. manually faking, fructose, glucose content are lower than 20%, and the content of sucrose is up to more than 20%, and what have even reaches more than 30%.
Table 1 sample size measurement result (%)
| Sample and numbering | Fructose | Glucose | Sucrose |
| No. 01 (acacia nectar) | 32.2 | 30.5 | 0.9 |
| No. 02 (acacia nectar) | 31.8 | 31.5 | 1.3 |
| No. 03 (acacia nectar) | 33.4 | 30.9 | 2.8 |
| 04 (commercially available) | 17.2 | 26.8 | 15.6 |
| 05 (commercially available) | 18.6 | 28.9 | 8.6 |
| 06 (commercially available) | 25.6 | 27.4 | 1.6 |
| 07 (commercially available) | 28.4 | 19.6 | 0.8 |
| 08 (commercially available) | 30.8 | 30.4 | 12.3 |
| 09 (commercially available) | 31.8 | 24.3 | 25.7 |
| 10 (commercially available) | 33.8 | 31.5 | 32.6 |
Claims (5)
1. an efficient liquid-phase chromatography method for rapidly quantifying honey quality, is characterized in that collecting representative honey sample 10 ~ 20 parts, takes appropriate amount of sample, with pure acetonitrile pre-treatment, detect for high performance liquid chromatography.With sugared dedicated analysis post for chromatographic column, acetonitrile-water (75: 25) is mobile phase.Detect with differential refraction detector, quantified by external standard method, calculate the content of glucose, fructose and sucrose.
2. chromatographic column is sugared dedicated analysis post (4mm × 250mm) according to claim 1.
3. chromatographic column column temperature is 35 DEG C according to claim 1.
4. mobile phase flow rate is 1ml/min according to claim 1.
5. mobile phase sample size is 10 μ L according to claim 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181403A (en) * | 2018-01-31 | 2018-06-19 | 安徽泓顺源生物科技有限公司 | A kind of efficient liquid-phase chromatography method of rapidly quantifying honey quality |
| CN110749663A (en) * | 2018-07-24 | 2020-02-04 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for identifying whether honey is doped with non-milk powder foreign protein |
| CN113820434A (en) * | 2021-11-23 | 2021-12-21 | 中国农业科学院蜜蜂研究所 | Method for identifying maturity of acacia honey |
| CN114088833A (en) * | 2021-11-17 | 2022-02-25 | 广州浩宇生物科技有限公司 | Method for rapidly detecting glucose content in food |
-
2014
- 2014-10-11 CN CN201410535926.0A patent/CN105572237A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108181403A (en) * | 2018-01-31 | 2018-06-19 | 安徽泓顺源生物科技有限公司 | A kind of efficient liquid-phase chromatography method of rapidly quantifying honey quality |
| CN110749663A (en) * | 2018-07-24 | 2020-02-04 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for identifying whether honey is doped with non-milk powder foreign protein |
| CN114088833A (en) * | 2021-11-17 | 2022-02-25 | 广州浩宇生物科技有限公司 | Method for rapidly detecting glucose content in food |
| CN113820434A (en) * | 2021-11-23 | 2021-12-21 | 中国农业科学院蜜蜂研究所 | Method for identifying maturity of acacia honey |
| WO2023093731A1 (en) * | 2021-11-23 | 2023-06-01 | 中国农业科学院蜜蜂研究所 | Method for identifying degree of maturity of acacia honey |
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