CN107589081A - A kind of anti-interference quick determination method of tealeaves China and foreign countries source doping sucrose - Google Patents
A kind of anti-interference quick determination method of tealeaves China and foreign countries source doping sucrose Download PDFInfo
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Abstract
The invention discloses a kind of anti-interference quick determination method of tealeaves China and foreign countries source doping sucrose, using PVPP activated carbon combine adsorption agent, removes tea sample extract solution mesostroma composition to resorcinol chromogenic reaction and the interference of detection.Specific method is included sample extraction, is carried out selective absorption removal, chromogenic reaction to the interference matrix in sample using adsorbent, color identifying is used to qualitatively judge or absorbance measuring is for quantitatively detecting four steps.Selective absorption wherein to matrix is the committed step for the interference free performance for realizing detection.The present invention is realized to the qualitative of the additional sucrose of tea processing process and quantitative quick measure, has the characteristics that strong antijamming capability, applied widely, simple to operate, reliable results, especially suitable for adulterating the fast qualitative examination of sucrose and quantitative detection in tealeaves.
Description
Technical field
The invention belongs to field of food detection, and in particular to the anti-interference quick detection of external source addition sucrose in a kind of tealeaves
Method.
Background technology
In recent years, to pursue the more preferable apparent quality of tealeaves, indivedual producers have when the phenomenon of sucrose is added in tealeaves
Occur.On the one hand the sucrose added during tea processing can be influenceed to the organoleptic quality into tea in fragrance, color and luster etc.
Judge；Simultaneously as, there is large effect the features such as easy moisture absorption of sucrose, perishable and easy breed bacteria to quality and safety of tea.
Thus, cause more and more extensive concern in tea quality supervisory system and consumer on sucrose addition, it is corresponding quick
Detection method needs as market.To adapt to this present situation, our early developments are a kind of to be based on sucrose hydrolysis and resorcinol
Sucrose rapid screening, the method for detection are added in being directed in tealeaves for chromogenic reaction, in order in Tea Production and the process of circulation
Monitoring in real time.
But in actual applications it was found that sucrose in the teas sample such as this method black tea higher to attenuation degree into
Go-on-go survey is sensitive reliable, and in the colour developing and detection process to green tea (particularly summer and autumn green tea), more serious interference be present and show
As：On the one hand, (1 under the conditions of the reaction solution of used highly acid：1 hydrochloric acid solution), fructose (sucrose hydrolysis generation) exists
Faint colour developing can spontaneously occur in itself with sample substrate (when being free of resorcinol colour reagent) in simple hydrochloric acid solution
Reaction, certain light red is presented in itself, and easily forms cotton-shaped muddiness, and interference color judges and absorbance measurement；It is and existing with this
As by contrast, in the test tubes containing colour reagent, some compositions in sample substrate disturb resorcinol and fructose
Reaction, on the contrary cause sugar composition can not normally develop the color, cause false negative testing result.
Thus, develop in a kind of tealeaves more pervasive, that Tea Samples matrix interference itself can be resisted and add sugarcane
The quick determination method of sugar, has obvious application value.
The content of the invention
It is an object of the invention to provide the anti-interference quick determination method that sucrose is adulterated in a kind of tealeaves, to be adapted to not
With the detection demand of teas sample.This method has strong antijamming capability, applied widely, easy to operate, detection is rapid, result
The features such as reliable.
To realize above-mentioned target, the present invention adopts the following technical scheme that：
A kind of anti-interference quick determination method of tealeaves China and foreign countries source doping sucrose, methods described are：
(1) Tea Samples water to be measured is extracted or brewed, and is removed tealeaf residue and is obtained millet paste sample to be measured；
(2) anti-interference process：Adsorbent will be added in millet paste sample to be measured, after mixing under normal temperature reaction or heating water bath 3
~30min, centrifugation, takes supernatant as testing sample solution；
(3) testing sample solution is qualitatively judged using resorcinol colour reagent and quantitatively detected；
The adsorbent is PVPP and quality of activated carbon than 1:0~1 mixing, therein 0 represents
Can be 0, that is, be not added with activated carbon, but preferred adsorbent be PVPP with quality of activated carbon than 1:0.1~0.5
Mixing, more preferably 1:0.2 mixing；The addition of adsorbent is to be calculated as 5~100mg/mL with the volume of millet paste sample to be measured,
It is preferred that 10~50mg/mL, more preferably 30mg/mL；
Further, in the step (1), millet paste sample to be measured is prepared by one of following three kinds of schemes：
(1-A) qualitatively judges for simple, and by Tea Samples to be measured, the mass ratio according to tea, water is 1：20~100 is (excellent
Select 1:50) add boiling water and brew 2~10min, leach millet paste as millet paste sample to be measured, then carry out the anti-interference of step (2)
Processing and the qualitative judgement of step (3)
(1-B) accurately weighs Tea Samples to be measured, the mass ratio according to tea, water is 1 for quantitative detection:10~50 is (excellent
Select 1:40) deionized water boiled, is added, ultrasonic extraction 2 times, each 5~10min of ultrasonic extraction, merging filtrate, after constant volume
To testing sample solution, the quantitative detection of the anti-interference process and step (3) of step (2) is then carried out；The volume of filtrate constant volume
50~200mL/g (preferably 100mL/g) is calculated as with the quality of tealeaves.
Further, after ultrasonic extraction Tea Samples, tealeaf residue is can wash by water, cleaning fluid is incorporated to filtrate, and then constant volume obtains
To testing sample solution.
(1-C) for that should qualitatively judge and the sample that further need to quantitatively detect, or need to qualitatively judge in advance and according to
Result is qualitatively judged to decide whether that the sample of detection need to be quantified, it is preferential to prepare millet paste sample to be measured from (1-B) method.
In the step (2), after adding adsorbent in millet paste sample to be measured, preferably 50 DEG C of water-baths, 10min is heated, then
Centrifuge, take supernatant as testing sample solution.
It is preferably in the step (3), the step of qualitative judgement：
(3-A1) prepares colour reagent：Resorcinol is dissolved in hydrochloric acid (preferably 18~20% salt of mass fraction 7~25%
Acid), it is made into 0.1~2.0g/L of resorcinol concentration solution；The concentration of wherein resorcinol is preferably 0.5g/L；
(3-A2) is qualitatively judged：Two test tubes, respectively test tube a, b are taken, are separately added into isometric colour reagent, then
The deionized water of same volume and testing sample solution is taken to be separately added into test tube a, b, deionized water or testing sample solution are with showing
The volume ratio of color reagent is 1：5~50, (preferably 1：10).Then two test tubes are immersed in boiling water bath simultaneously, reacts 2~10min
After take out test tube, with water rinse cooling after contrast liquid color in two test tubes, using test tube a colors as reference, if test tube b in occur
It is obvious red, then it is determined as the positive, that is, sucrose is doped with surveyed tealeaves；If not occurring obvious red in test tube b, it is determined as
Feminine gender, sucrose is not added with tealeaves.
In the step (3), quantitatively the step of detection is preferably：
(3-B1) prepares colour reagent：Resorcinol is dissolved in hydrochloric acid (preferably 18~20% salt of mass fraction 7~25%
Acid), 0.1~2.0g/L of resorcinol concentration solution is made into, the concentration of the resorcinol is preferably 0.5g/L；
(3-B2) prepares sucrose standard solution：Pure sucrose sample is analyzed with deionized water dissolving, prepares more than 3 kinds respectively not
Aqueous sucrose solution with concentration is as standard liquid, 0.01~5g/L of concentration range of sucrose standard solution；
(3-B3) drawing curve：The test tube of respective numbers is taken according to foregoing prepared sucrose standard solution number, is compiled
Number record；Respectively by deionized water and sucrose standard solution and colour reagent according to volume ratio 1：10~100 (preferably 1：30)
The test tube of reference numeral is added, and mixing shakes up respectively, takes out after 80~100 DEG C of 1~10min of heating water bath, is rushed immediately with water
Wash and be cooled to room temperature, under 400~500nm wavelength conditions, using test tube solution where foregoing deionized water as reference solution, use
The absorbance of sucrose solution in each test tube of spectrophotometric determination；Then using the concentration of sucrose standard solution as abscissa, corresponding
Absorption values be ordinate, drawing curve simultaneously fits to obtain calibration curve equation；
(3-B4) actual sample determines：According to testing sample quantity, the test tube and number record of respective numbers are taken, in test tube
Be separately added into respective sample numbering, treat with deionized water in test tube in step (3-B3) or sucrose standard solution same volume
Sample solution is surveyed, and adds the colour reagent with same volume in each test tube in step (3-B3), according to step (3- after mixing
B3) identical method heating water bath, spectrophotometer detection, are still detected using reference solution used in step (3-B3) as this
Reference solution, using the absorbance of solution in each test tube of spectrophotometric determination, then according to step (3-B3) standard curve
Equation, conversion obtain the sucrose concentration in corresponding testing sample solution, and combine the sample quality in foregoing pre-treatment step and
Extracting liquid volume relation after constant volume, the content that sucrose is adulterated in corresponding tealeaves to be measured is calculated.
In the quantitative detecting step (3-B3), the volume ratio of sucrose standard solution and colour reagent is preferably 1:30；
In step (3-B3), bath temperature is preferably 100 DEG C, and the heating water bath time is preferably 4min, spectrophotometer
Detection wavelength is preferably 485nm.
The present invention anti-interference Cleaning Principle be：It is more highly concentrated when existing in Tea Samples extract solution according to this experimental study
During the catechin component of degree, serious interference can be caused in itself to resorcinol chromogenic reaction；In addition, in extract solution
Other colored components are to the detection process after colour developing --- and larger do be present in the process particularly with the naked eye qualitatively judged
Disturb, have impact on the reliability of direct result of determination.PVPP and activated carbon have to above two interference respectively
Certain removal effect, therefore in this method, using PVPP-activated carbon combine adsorption agent, effectively eliminate
Foregoing two class interference matrix in tea extract.After anti-interference process, the sucrose in tea extract is in hydrochloric acid
Under the conditions of occur hydrolysis, generate the glucose of a molecule and the fructose of a molecule；Fructose tries under the conditions of hydrochloric acid with colour developing
The chromogenic reaction of high selectivity occurs for the resorcinol in agent, generates cherry product, product has maximum suction near 485nm
Receive, thus the qualitative discrimination for carrying out adulterating sucrose respectively in tealeaves with absorption values can be identified according to reacted solution colour
With quantitative detection, so as to solve in green tea adulterate sucrose quick determination method in Problem of False Negative；Meanwhile this anti-interference side
Method eliminates the color background of testing sample solution in acid condition in itself, avoids special reference solution during absorbance measurement
Configuration and use, it is not necessary to each sample individually prepares the reference solution of the sample, but all samples are adopted
With identical reference, it thereby simplify absorbance measurement and operate and reduce concentrated hydrochloric acid dosage, thus for youngsters such as black tea
The detection of the relatively low fermentation teas of catechin content similarly has actual application value.
The anti-interference quick determination method of sucrose has following technical characterstic in the tealeaves of the present invention：
Quickly qualitatively judged and fixed 1. the present invention can realize to tea processing process or into the sucrose artificially added in tea
Amount detection.Method effectively eliminates interference of the Tea Samples matrix to detection, applied widely, available for through everfermentation or not sending out
The Tea Samples of all teas of ferment technique processing；And half-quantitative detection is not required to by any detection device, naked eyes
Judge；Real-time, quick, Site Detection can be realized, can the characteristics of circulating suitable for the current tealeaves in China and sell relative distribution
Quality monitoring for sales of tea end.
2. compared with conventional liquid chromatogram or LC-MS-MS, this method instrument is simple, right
The professional level of operator requires low, avoids detection process to large-scale instrument and the heavy dependence of specialized laboratory, and can
Significantly improve detection efficiency, suitable for China's Tea Production and circulation relative distribution the characteristics of, to tealeaves actual production, circulation and
Monitor procedure is respectively provided with application value.
In summary, the present invention is intended to provide a kind of be directed in current Tea Industry present situation artificially adulterates the anti-of sucrose problem
Fast Detection Technique is disturbed, technical support is provided for the quality safety management of Tea Industry.This method can it is rapidly qualitative or
Person's quantitatively sucrose doping situation in determination sample.
Brief description of the drawings
The green tea sample of Fig. 1 (B, C, D) 3% cane sugar contents after (A) before anti-interference process qualitatively judges experimental phenomena pair
Than figure.Wherein, A figures are without anti-interference process, and B figures are to add activated carbon processing, and C figures are to add PVPP
Processing, D figures are to add PVPP and active carbon mixed adsorbent processing.
Fig. 2 adsorbent amounts influence result figure to the detection rate of recovery that sucrose is added during tea processing.Wherein insert
The test tube photo entered is the green tea sample colour developing result photo under the conditions of three different adsorbent amounts.
Fig. 3 millet paste recovery of standard addition experimental result after anti-interference process.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention
Technical scheme is described further, but protection scope of the present invention not limited to this.
Embodiment 1
Different sorbent treatment Contrast on effect experiments
1) weigh after resorcinol 0.10g is dissolved in 100mL concentrated hydrochloric acids, mixed with 100ml deionized waters, be made into colour developing examination
Agent；
2) the green tea sample 3.0g of 3% cane sugar content of the advance frying in laboratory is weighed, boiling water 150ml is added and brews
5min, millet paste is leached, as millet paste to be measured.
3) above-mentioned each four parts of millet paste sample 1ml is taken, is respectively placed in the centrifuge tube of 4 numberings, centrifuge tube 1 is added without absorption
Agent, centrifuge tube 2 add 30mg activated carbons, and centrifuge tube 3 adds 30mg PVPPs, and centrifuge tube 4 adds 25mg and handed over
Join polyvinylpyrrolidone and 5mg activated carbons；
50 DEG C of heating water bath 10min after mixing, centrifugation；
4) the clear glass test tube of 8 same sizes is taken, wherein 4 each addition 1ml hydrochloric acid solution (concentrated hydrochloric acid and deionizations
Water volume ratio 1:1 is mixed to get), it is calculated as A1, B1, C1, D1 pipe；Other four each to add 1ml colour reagents, be calculated as A2, B2,
C2, D2 are managed.The supernatant of 0.1ml centrifuge tubes 1 is separately added into A1 and A2 pipes；Be separately added into B1 and B2 pipes 0.1ml from
The supernatant of heart pipe 2；The supernatant of 0.1ml centrifuge tubes 3 is separately added into C1 and C2 pipes；It is separately added into D1 and D2 pipes
The supernatant of 0.1ml centrifuge tubes 4；
5) above-mentioned 8 test tubes are immersed in boiling water bath simultaneously and heated, taken out simultaneously after about 5min, it is cold that running water rinses test tube
But after, experimental result photo is as shown in fig. 1；
Include sample-hydrochloric acid background color situation (left bottle) and sample-resorcinol in every group of two vials respectively
The result that develops the color (right bottle)；It is determined as that sucrose addition is positive when right bottle is compared with left bottle color, is presented obvious red, is otherwise the moon
Property.Compared with other group of phenomenon, D group background colors are minimum, and colour developing result is the most obvious, and antijamming capability is most strong；D groups are obvious
It is consistent with sample actual conditions for positive test symbol；B, two groups of color discrimination reliabilities of C are weaker than D groups, show the anti-of pre-treatment
Interference performance is poor；And false negative result is presented due to the interference of tealeaves matrix in A groups.Therefore, in general, it is poly- using crosslinking
The anti-jamming effectiveness of vinylpyrrolidone and active carbon mixed adsorbent is optimal.
The influence of embodiment 2, adsorbent amount to the millet paste sample color developing effect containing sucrose
1) black tea, each 1.0g of green tea sample for weighing addition sucrose in process respectively are respectively placed in conical flask, respectively
About 40mL boiling water is added, conical flask is put into ultrasonic extraction 5min in processor for ultrasonic wave；After filtering out extract solution, boiling water is added again
40mL, repeat above-mentioned supersound process.Respective tea grounds is cleaned with deionized water twice, and the ultrasound twice for merging same Tea Samples carries
Liquid and tea grounds cleaning fluid are taken, 100mL is settled to after cooling, as millet paste sample.
2) 7 centrifuge tubes are taken, are respectively put into above-mentioned each 1mL of gained black tea infusion sample, and sequentially add different quality
Adsorbent, adsorbent are PVPP and quality of activated carbon ratio 1:0.2 mixing, heating water bath after mixing
10min, centrifuge, take supernatant as black tea testing sample solution (7)；Processing green tea millet paste sample is operated with identical, obtained
To 7 green tea testing sample solutions through different adsorbent amount anti-interference process.
3) pure sucrose sample is analyzed with deionized water dissolving, prepares 0,0.05,0.10,0.30,0.50g/L concentration respectively
Sucrose solution is as standard liquid.
4) weigh after resorcinol 0.10g is dissolved in 100mL concentrated hydrochloric acids, mixed with 100ml deionized waters, be made into colour developing examination
Agent；
5) 5 test tubes that numbering is S0#~S4# are taken, sequentially add sucrose standard solution that 0.2mL steps 3) are prepared and
The colour reagent that 6mL steps 4) are prepared, after mixing, takes out after heating 4min in boiling water bath, is rinsed be cooled to water immediately
Room temperature；Under 485nm wavelength conditions, using S0# test tube solutions as reference solution, spectrophotometric determination S1#~S4# test tubes are used
The absorbance of middle liquid；Then it is ordinate by abscissa, corresponding absorption values of the concentration of sucrose standard solution, draws
Working curve simultaneously fits to obtain calibration curve equation；
6) numbering 1#~14# 14 test tubes are taken, sequentially add each 0.2mL of testing sample solution obtained by step 2),
And the colour reagent that 6mL steps 4) are prepared respectively is added, after mixing, 4min is heated in boiling water bath, test tube is taken out and uses immediately
Water rinses and is cooled to room temperature；Under 485nm wavelength conditions, still using S0# test tube solutions as reference solution, measured using spectrophotometric
Determine the absorbance of liquid in 1#~14# test tubes；Then according to the calibration curve equation of step 5), corresponding testing sample is calculated
Sucrose concentration in solution, and the extracting liquid volume relation after the sample quality and constant volume in foregoing pre-treatment step is combined, meter
Calculate and obtain the content that sucrose is adulterated in corresponding tealeaves to be measured；According to the sucrose amount added in sample processing procedure, conversion obtains
The corresponding rate of recovery.Specific experiment result is as shown in Figure 2.
It can be seen that after carrying out millet paste sample anti-interference process using adsorbent, there is necessarily the rate of recovery of sucrose in black tea sample
Raising；The sucrose detection rate of recovery in green tea sample is then significantly increased, and brings up to 101% from -76%, detection performance is obvious
Enhancing；Cumulated volume experimental result and the detection to millet paste matrix, finally selected 30mg/mL is optimum absorbent dosage.
Embodiment 3, recovery of standard addition experiment
By the condition reagent preparation and black tea of previous embodiment 2, green tea blank millet paste sample, and drawing curve.
In two kinds of millet paste samples of gained, respectively make the sucrose addition of 0,0.05,0.10,0.20,0.30,0.60g/L five concentration level, inhale
Attached dose with embodiment 2, adsorbent amount is 30mg/1mL millet paste samples；And determine the rate of recovery of detection method.Experimental result shows
Show, under 0.05~0.60g/L mark-on level, method to the detection rate of recovery of sucrose in black tea infusion for 103.4%~
117.8%, the detection rate of recovery to sucrose in green tea millet paste is 91.9%~100.5%.
Spiked levels level in above-mentioned millet paste is converted to cane sugar content in dry tea and mapped in Excel, is fitted to obtain sugarcane
Linear equation between sugared addition and detected level is y=1.0022x+0.52 (R2=0.9985), concrete outcome such as Fig. 3 institutes
Show.Thus result understands that method provided by the present invention is consistent to different black tea, green tea matrix responding to height, it was demonstrated that this
Method antijamming capability excellent in sucrose detection.
Embodiment 4, two Tea Samples (numbering is sample 1 and sample 2) are carried out with sucrose doping qualitative discrimination
1) colour reagent is prepared by the condition of previous embodiment 2；
2) Tea Samples 3.0g to be measured is weighed respectively, boiling water 150ml is added and brews 5min, leaches millet paste as millet paste sample
1 and millet paste sample 2.
3) above-mentioned 2 each 1ml of millet paste sample 1 and millet paste sample is taken respectively, is placed in centrifuge tube, it is each to add 30mg adsorbents
(adsorbent is PVPP and quality of activated carbon ratio 1:0.2 mixing), heating water bath 10min after mixing, from
The heart, respectively take supernatant 0.1mL to add in cuvette and (be calculated as test tube a and b respectively), separately take test tube add 0.1mL go from
Sub- water, it is calculated as test tube c.1mL colour reagents are respectively added in above-mentioned three test tubes, are mixed.
4) above-mentioned three test tubes are immersed in boiling water bath simultaneously and heated, taken out simultaneously after about 5min, running water rinses test tube
After cooling, using c as standard, a, the color of b test tubes are contrasted respectively.Compared with test tube c, find occur obvious red in test tube a, say
Bright corresponding Tea Samples 1 are positive, i.e., are doped with sucrose in Tea Samples 1；And solution colour can without naked eyes in test tube b
Show color, therefore judge to know in its corresponding Tea Samples 2 undoped with sucrose.
The quantitative detection of cane sugar content is adulterated in embodiment 5, tealeaves
1) by the step 1) of previous embodiment 2 condition extraction millet paste sample, and according to the step 3) of embodiment 2,4), 5) draw
Working curve, it is y=5.0143x+0.0091 (R that fitting, which obtains working curve equation, in Excel2=0.9986).
2) take step 1) to extract millet paste sample 1mL and add the centrifuge tube for being put into 30mg adsorbents in advance, 50 DEG C after shaking up
Heating water bath 10min；Centrifugation, takes supernatant 0.2mL in teat glass, and after adding 6mL colour reagents, test tube is put into boiling water
4min is heated in bath.
3) take out test tube and rinsed in the case where flowing running water and be cooled to room temperature.Under 485nm wavelength conditions, with bent with work
Line number according to surveying and determination when identical reference solution as reference, determine the absorbance of liquid in test tube.Bring absorbance data into step
Rapid 1) gained working curve, is calculated in each sample corresponding sucrose addition (with dry tea percentages).Experimental result is such as
Table 1 below：
Table 1
Claims (10)
1. a kind of anti-interference quick determination method of tealeaves China and foreign countries source doping sucrose, it is characterised in that methods described is：
(1) Tea Samples water to be measured is extracted or brewed, and is removed tealeaf residue and is obtained millet paste sample to be measured；
(2) anti-interference process：Adsorbent will be added in millet paste sample to be measured, after mixing under normal temperature reaction or heating water bath 3~
30min, centrifugation, takes supernatant as testing sample solution；
(3) testing sample solution is qualitatively judged using resorcinol colour reagent and quantitatively detected；
The adsorbent is PVPP and quality of activated carbon than 1:0~1 mixing, therein 0 represent can be with
For 0, that is, it is not added with activated carbon；The addition of adsorbent is to be calculated as 5~100mg/mL with the volume of millet paste sample to be measured.
2. the method as described in claim 1, it is characterised in that the adsorbent is PVPP and activated carbon
Mass ratio 1:0.1~0.5 mixing.
3. method as claimed in claim 2, it is characterised in that the adsorbent is PVPP and activated carbon
Mass ratio 1:0.2 mixing.
4. the method as described in claim 1, it is characterised in that the addition of the adsorbent is with the body of millet paste sample to be measured
Product is calculated as 10~50mg/mL.
5. the method as described in claim 1, it is characterised in that in the step (1), millet paste sample to be measured presses following three kinds of sides
It is prepared by one of case：
(1-A) qualitatively judges for simple, and by Tea Samples to be measured, the mass ratio according to tea, water is 1：20~100 add boiling water
Brew 2~10min, leach millet paste as millet paste sample to be measured, then carry out the anti-interference process and step (3) of step (2)
Qualitatively judge；
(1-B) accurately weighs Tea Samples to be measured, the mass ratio according to tea, water is 1 for quantitative detection:10~50, addition is boiled
The deionized water of boiling, ultrasonic extraction 2 times, each 5~10min of ultrasonic extraction, merging filtrate, it is molten that testing sample is obtained after constant volume
Liquid, then carry out the quantitative detection of the anti-interference process and step (3) of step (2)；
(1-C) is for that should qualitatively judge and the sample that further need to quantitatively detect, or need in advance qualitatively judge and be sentenced according to qualitative
Determine result to decide whether that the sample of detection need to be quantified, it is preferential to prepare millet paste sample to be measured from (1-B) method.
6. the method as described in claim 1, it is characterised in that in the step (2), adsorbent is added in millet paste sample to be measured
Afterwards, 50 DEG C of water-baths, 10min is heated, is then centrifuged for, takes supernatant as testing sample solution.
7. the method as described in claim 1, it is characterised in that be in the step (3), the step of qualitative judgement：
(3-A1) prepares colour reagent：Resorcinol is dissolved in the hydrochloric acid of mass fraction 7~25%, is made into resorcinol concentration
0.1~2.0g/L solution；
(3-A2) is qualitatively judged：Two test tubes, respectively test tube a, b are taken, isometric colour reagent is separately added into, then takes phase
The deionized water and testing sample solution of same volume are separately added into test tube a, b, and deionized water or millet paste sample to be measured try with colour developing
The volume ratio of agent is 1：5~50, then two test tubes are immersed in boiling water bath simultaneously, test tube is taken out after reacting 2~10min, uses water
Liquid color in two test tubes is contrasted after rinsing cooling, using test tube a colors as reference, if appearance is obvious red in test tube b, is judged
For the positive, that is, sucrose is doped with surveyed tealeaves；If not occurring obvious red in test tube b, it is determined as feminine gender, does not add in tealeaves
Add sucrose.
8. the method as described in claim 1, it is characterised in that in the step (3), quantitatively the step of detection is：
(3-B1) prepares colour reagent：Resorcinol is dissolved in the hydrochloric acid of mass fraction 7~25%, is made into resorcinol concentration 0.1
~2.0g/L solution；
(3-B2) prepares sucrose standard solution：Pure sucrose sample is analyzed with deionized water dissolving, it is dense to prepare more than 3 kinds differences respectively
The aqueous sucrose solution of degree is as standard liquid, 0.01~5g/L of concentration range of sucrose standard solution；
(3-B3) drawing curve：The test tube of respective numbers, numbering note are taken according to foregoing prepared sucrose standard solution number
Record；Respectively by deionized water and sucrose standard solution and colour reagent according to volume ratio 1：10~100 add reference numeral
Test tube, and mixing shakes up respectively, is taken out after 80~100 DEG C of 1~10min of heating water bath, is rinsed with water be cooled to room temperature immediately,
Under 400~500nm wavelength conditions, using test tube solution where foregoing deionized water as reference solution, spectrophotometric determination is used
The absorbance of sucrose solution in each test tube；Then it is by abscissa, corresponding absorption values of the concentration of sucrose standard solution
Ordinate, drawing curve simultaneously fit to obtain calibration curve equation；
(3-B4) actual sample determines：According to testing sample quantity, the test tube and number record of respective numbers are taken, in test tube respectively
Testing sample solution that respective sample is numbered, with sucrose standard solution same volume in test tube in step (3-B3) is added, and
The colour reagent with same volume in each test tube in step (3-B3) is added, according to step (3-B3) identical method water after mixing
Bath heating, spectrophotometer detection, the reference solution still detect using reference solution used in step (3-B3) as this, using divide
The absorbance of solution in each test tube of light photometric determination, phase is then obtained according to step (3-B3) calibration curve equation, conversion
The sucrose concentration in testing sample solution is answered, and combines the extracting liq after the sample quality and constant volume in foregoing pre-treatment step
Product relation, the content that sucrose is adulterated in corresponding tealeaves to be measured is calculated.
9. the method as described in claim 1, it is characterised in that in the quantitative detecting step (3-B3), sucrose standard solution with
The volume ratio of colour reagent is 1:30.
10. the method as described in claim 1, it is characterised in that in the quantitative detecting step (3-B3), bath temperature 100
DEG C, the heating water bath time is 4min, and the Detection wavelength of spectrophotometer is 485nm.
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| CN201710595014.6A CN107589081B (en) | 2017-07-20 | 2017-07-20 | Anti-interference rapid detection method for exogenous sucrose-doped tea |
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| CN201710595014.6A CN107589081B (en) | 2017-07-20 | 2017-07-20 | Anti-interference rapid detection method for exogenous sucrose-doped tea |
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| CN201710595014.6A Active CN107589081B (en) | 2017-07-20 | 2017-07-20 | Anti-interference rapid detection method for exogenous sucrose-doped tea |
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Cited By (1)
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| CN110044887A (en) * | 2019-04-24 | 2019-07-23 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A kind of method of quick differentiation normal tealeaves and suspicious tealeaves |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044887A (en) * | 2019-04-24 | 2019-07-23 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A kind of method of quick differentiation normal tealeaves and suspicious tealeaves |
| CN110044887B (en) * | 2019-04-24 | 2022-04-08 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Method for rapidly distinguishing normal tea leaves and suspicious tea leaves |
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| CN107589081B (en) | 2020-05-08 |
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