CN109001341A - A kind of high performance liquid chromatography, which quickly detects, adulterates sucrose in tealeaves - Google Patents
A kind of high performance liquid chromatography, which quickly detects, adulterates sucrose in tealeaves Download PDFInfo
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- CN109001341A CN109001341A CN201811153529.1A CN201811153529A CN109001341A CN 109001341 A CN109001341 A CN 109001341A CN 201811153529 A CN201811153529 A CN 201811153529A CN 109001341 A CN109001341 A CN 109001341A
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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
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Abstract
It is quickly detected the invention discloses a kind of high performance liquid chromatography and adulterates sucrose in tealeaves, accurate quantitative analysis measurement is carried out to the sucrose that adulterates in tealeaves using high performance liquid chromatograph, key step includes: to detect the pretreatment of sample, measurement.High performance liquid chromatography has the characteristics that separative efficiency is high, analysis speed is fast, detection sensitivity is high and has wide range of applications, particularly suitable for higher boiling, macromolecular, highly polar and poor thermal stability compound separation analysis.According to existing laboratory condition, it is contemplated that easy to operate, reliable and stable, failure rate is low.Further according to the property of sucrose, in ultra-violet (UV) band without absorption, but there is certain index of refraction, therefore selected the high performance liquid chromatograph equipped with differential refraction detector.The present invention is realized to the qualitative of the additional sucrose of tea processing process and quantitative quickly measurement, have the characteristics that instrument is simple, testing cost is low, high sensitivity, the professional level of operator is required low, the characteristics of suitable for China's Tea Production and circulation relative distribution, there is application value in Tea Production, circulation and monitor procedure.
Description
Technical field
The invention belongs to field of food detection, and in particular to a kind of high performance liquid chromatography, which quickly detects, adulterates sugarcane in tealeaves
Sugar.
Background technique
Sucrose and sucrose solution can generate a variety of different chemical reactions under the action ofs heat, acid, alkali, yeast etc..Reaction
Result not only directly contribute the loss of sucrose, but also some pairs of harmful substances of sugaring can be generated.Candy is heated to
160 DEG C, it can thermally decompose and just be melted into thick transparent liquid, be crystallized again when cooling.Extending heating time, sucrose divide
Solution is glucose and anhydrofructose.Under 190-220 DEG C of higher temperature, just dehydrating condensation becomes caramel to sucrose.Caramel is into one
Step heating then generates the products such as carbon dioxide, carbon monoxide, acetic acid and acetone.Under humid conditions, sucrose is in 100 DEG C of time-divisions
Solution, releases moisture, color blackening.Sucrose solution through a long time ebuillition of heated under normal pressure, the sucrose of dissolution, which will be slow, to be decomposed into
The glucose and fructose of equivalent, i.e. generation transformation.If sucrose solution is heated to 108 DEG C or more, hydrolysis is rapid, sugar juice
Concentration is bigger, and hydrolysis is more significant.Metal material used in water boiling supply also has an impact to sucrose inversion rate.Such as: sugarcane
Transformation of the sugar juice in bronze, brass or copper ware, more than big in silverware, glass container is almost without what influence.
During Tea Production, some tea growers are to promote quality, and a certain amount of sucrose is often added in tealeaves, with
This improves sugared content in tealeaves, and still, tealeaves can have many problems after this sugaring processing, for example, patients with diabetes mellitus
Afterwards, meeting making patients' state of an illness seriously affects product in addition, the tealeaves of sugaring processing is often apt to deteriorate mouldy during storage
Matter.Therefore, it carries out detection for sucrose addition in tealeaves to need to take seriously, still, detection method has profession mostly now
Restricted, many detection methods, which require professional person, to be carried out, and do not have spectrum.Therefore it provides a kind of simple and feasible
Efficient tealeaves in sucrose detection method it is necessary.
Summary of the invention
It can quickly determine to adulterate sucrose in tealeaves under the conditions of simple device the purpose of the present invention is to provide one kind
Detection method, this method have the distinguishing features such as easy to operate, equipment is simple, detection time is short.
To realize above-mentioned target, the present invention adopts the following technical scheme:
A kind of high performance liquid chromatography, which quickly detects, adulterates sucrose in tealeaves, the method includes qualitatively judging and quantitative detection,
In the tealeaves adulterate sucrose qualitative judgement method the following steps are included:
(1) sample pretreatment: Tea Samples being placed in 65 DEG C of baking ovens and are dried for 24 hours to constant weight, damp-proof treatment, crushed into powder, until
60 mesh sieve can be crossed.
(2) sample pretreatment: accurately weigh 5g(and be accurate to 0.01 g) sample to 50 mL have plug plastics graduated centrifuge tube
In, it is settled to scale with water, is mixed, it is accurate to inhale to be centrifuged 10min not less than 3000 r/min after ultrasound extracts 10 min
It takes 5.00 m L of supernatant in another 10 mL volumetric flask, is settled to scale with acetonitrile, mix.Through 0.45 μm of miillpore filter
After filtering, to liquid chromatogram measuring.
(3) it measures :(a) high-efficient liquid phase chromatogram condition: chromatographic column: 5 μm of carbohydrate analysis column, the mm of 250 mm × 4.6
(i.d).Mobile phase: acetonitrile+water (volume ratio 4: 1)；Flow velocity: 1.5 m L/min；Column temperature: 30 DEG C；Sample volume: 15 μ L；Detection
Device pond temperature: 35 DEG C.
(b) Specification Curve of Increasing: accurate to draw 0.2 m L of sucrose standard stock solution, 1.0 m L, 2.0 m L, 4.0 m
L, 8.0 m L is settled to 10 m L with acetonitrile solution (volume ratio 1: 1), and the mass concentration of this standard series is 0.5 mg/
m L,2.5 mg/m L,5.0 mg/m L,10.0 mg/m L,20.0 mg/m L.Through 0.45 μm of filtering with microporous membrane, concentration
Sample introduction from low to high, using peak area as ordinate, draws standard curve using mass concentration as abscissa.
(d) quantitative determine: sucrose response should exceed the linear model of concentration in the standard curve range of linearity in the sample solution to be tested
It encloses, sample introduction is analyzed again after should diluting.
(e) result calculates: cane sugar content is calculated as the following formula in sample
Claims (10)
1. a kind of high performance liquid chromatography quickly detect in tealeaves adulterate sucrose method, it is characterised in that the method includes with
Lower step:
(1) sample pretreatment: Tea Samples being placed in 65 DEG C of baking ovens and are dried for 24 hours to constant weight, damp-proof treatment, crushed into powder, until
60 mesh sieve can be crossed.
2. (2) sample pretreatment: accurately weighing 5g (being accurate to 0.01g) sample and have in plug plastics graduated centrifuge tube to 50mL, use
Water is settled to scale, mixes, after ultrasound extracts 10min, to be centrifuged 10min, accurate Aspirate supernatant not less than 3000r/min
5.00m L is settled to scale in another 10mL volumetric flask, with acetonitrile, mixes.
3. after 0.45 μm of filtering with microporous membrane, to liquid chromatogram measuring.
4. (3) measuring: (a) high-efficient liquid phase chromatogram condition: chromatographic column: 5 μm of carbohydrate analysis column, 250mm × 4.6mm
(i.d)。
5. mobile phase: acetonitrile+water (volume ratio 4: 1)；Flow velocity: 1.5m L/min；Column temperature: 30 DEG C；Sample volume: 15 μ L；Detector
Pond temperature: 35 DEG C.
(6. b) Specification Curve of Increasing: accurate to draw sucrose standard stock solution 0.2m L, 1.0m L, 2.0m L, 4.0m L, 8.0m
L is settled to 10m L with acetonitrile solution (volume ratio 1: 1), and the mass concentration of this standard series is 0.5mg/m L, 2.5mg/m
L、5.0mg/m L、10.0mg/m L、20.0mg/m L。
7. concentration from low to high sat using mass concentration as abscissa with peak area to be vertical by sample introduction through 0.45 μm of filtering with microporous membrane
Mark draws standard curve.
8. (d) is quantitative determined: sucrose response should exceed the concentration range of linearity in the standard curve range of linearity in the sample solution to be tested
Sample introduction is analyzed again after should then diluting.
9. (e) result calculates: cane sugar content is calculated as the following formula in sample.
10.
In formula: the content of sucrose in X- sample, unit g/100g；
The mass concentration of sucrose, unit mg/mL in the sample liquid that C- is obtained by standard curve；
The last constant volume of V- sample liquid, unit mL；
M- sample quality, unit g；
F- extension rate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811153529.1A CN109001341A (en) | 2018-09-30 | 2018-09-30 | A kind of high performance liquid chromatography, which quickly detects, adulterates sucrose in tealeaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811153529.1A CN109001341A (en) | 2018-09-30 | 2018-09-30 | A kind of high performance liquid chromatography, which quickly detects, adulterates sucrose in tealeaves |
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| CN109001341A true CN109001341A (en) | 2018-12-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811153529.1A Pending CN109001341A (en) | 2018-09-30 | 2018-09-30 | A kind of high performance liquid chromatography, which quickly detects, adulterates sucrose in tealeaves |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109870519A (en) * | 2019-02-19 | 2019-06-11 | 中国农业科学院茶叶研究所 | A kind of detection method characterizing sucrose doped level in tealeaves using sucrose and fructose conversion content |
-
2018
- 2018-09-30 CN CN201811153529.1A patent/CN109001341A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109870519A (en) * | 2019-02-19 | 2019-06-11 | 中国农业科学院茶叶研究所 | A kind of detection method characterizing sucrose doped level in tealeaves using sucrose and fructose conversion content |
| CN109870519B (en) * | 2019-02-19 | 2022-10-18 | 中国农业科学院茶叶研究所 | Detection method for representing sucrose doping level in tea by using reduced content of sucrose and fructose |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181214 |
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| WD01 | Invention patent application deemed withdrawn after publication |