CN106501408A - A kind of honey adulteration detection method based on HPLC ELSD and partial least squares discriminant analysis method - Google Patents
A kind of honey adulteration detection method based on HPLC ELSD and partial least squares discriminant analysis method Download PDFInfo
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Abstract
The invention discloses a kind of honey adulteration detection method based on HPLC ELSD and partial least squares discriminant analysis method, belongs to technical field of food detection.The inventive method includes simple sample pretreatment, compound sugar and its isomer component in the method analysis purity honey of Evaporative light scattering detector (HILIC ELSD) and the honey sample mixed with HFCS or malt syrup is separated using hydrophilic Interaction Chromatography, and using pure honey and the difference of the oligomeric saccharic composition finger-print of adulterated honey, data processing is carried out by partial least squares discriminant analysis method and then realizes adulterated discriminating.This method can successfully identify HFCS incorporation more than 10%, the adulterated honey sample that malt syrup incorporation is more than 5%.For the adulterated honey of C4 plant sources syrup or C3 plant source syrup, the method can effectively differentiate that analytical instrument used is compared with popularization, easy to utilize.
Description
Technical field
The present invention relates to a kind of honey adulteration detection method based on HPLC-ELSD and partial least squares discriminant analysis method,
Belong to technical field of food detection.
Background technology
Used as natural materials, with unique local flavor, mouthfeel and nutritive value, main component is glucose and fruit to honey
Sugar, contains vitamin, multiple organic acids, inorganic salts, mineral matter and trace element simultaneously, and with functions of intestines and stomach is improved, raising is exempted from
The effects such as epidemic disease power, while also in empyrosis, prevention of cardiovascular disease, promote the aspects such as ulcer, wound healing to have preferably
Curative effect.In recent years, the nutritive value and health-care effect of honey is gradually known, both at home and abroad for the demand of honey
Constantly increasing, the yield of honey is difficult to meet the growing market demand so that drive of some illegal retailers in interests
Make down, mix the spurious with the genuine, adulterate by mixing the mode such as sweet substance such as honey, syrup at a low price, increase honey output.This is serious
Honey market order has been upset, the interests of regular beekeeper and enterprise have been compromised.
For the honey adulteration phenomenon of more generally existing, current domestic and international application is more universal and relatively effectively differentiates inspection
The adulterated LC-MS/MS authentication methods of survey method, i.e. stable carbon isotope rule of three and rice syrup, instrument costly,
It is difficult to popularize, and C4 plants syrup or a kind of adulterated honey in C plant syrup can only be differentiated, it is impossible to while differentiates this
Two kinds of syrup are adulterated, have its limitation.
Content of the invention
It is an object of the invention to provide a kind of honey adulteration for mixing starch syrup (including HFCS or malt syrup)
New detecting method, the method are not only suitable for C4 plant source syrup and are also applied for the adulterated honey discriminating of C3 plant source syrup.
For solving above-mentioned technical problem, the technical scheme is that：After sample is through water-soluble, filtration treatment, using hydrophilic
The method of action chromatography separation-Evaporative light scattering detector (HILIC-ELSD) analyzes pure honey and mixed with HFCS, malt
Compound sugar and its isomer component in the honey sample of syrup, and using pure honey and the oligomeric saccharic composition fingerprint of adulterated honey
The difference of collection of illustrative plates, carries out data processing by partial least squares discriminant analysis method and then realizes adulterated discriminating.
Technical scheme specifically includes the following steps：
1) first compound sugar in different sources, the pure honey sample in different nectar sources and its isomers are analyzed, are obtained
Arrive its characteristic finger-print, will several different sources, honey sample water dissolves constant volume and the filtration in different nectar source, then
High performance liquid chromatography separation and Evaporative light scattering detector are carried out to them, is determined according to the relative retention time of gained finger-print
Gained chromatographic data is imported the compound sugar standard colour chart fingerprint image that finger-print special-purpose software obtains honey by common characteristic peaks
Compose and determine its common characteristic peaks；
2) the compound sugar finger-print for obtaining honey sample to be checked is determined；
3) by step 2) the relative peak area data of the finger-print of honey sample to be checked that obtain and step 1) obtain
Several different sources, the relative peak area data composition matrix of the finger-print of the pure honey sample in different nectar sources, are carried out
Partial least squares discriminant analysis.
One embodiment of the present invention, specifically includes the following steps：
(1) pretreatment of honey sample to be checked
Sample pretreatment：1-2g honey samples to be checked are weighed in 25mL or 50mL volumetric flasks, distilled water constant volume fully shakes
Be shaken to mixed even after, take 1mL and cross 0.45 μm of miillpore filter, filtrate is used for the HPLC analyses of compound sugar and its isomers；
(2) honey sample to be checked, the liquid-phase chromatographic analysis of compound sugar mixed sample
Chromatographic condition：Chromatographic column is 3.5 μm of 4.6 × 250mm of XBridgeTMAmide；Mobile phase A is 50% acetonitrile, stream
Dynamic phase B is 75% acetonitrile, binary gradient elutes, Gradient program：0～20min, 0～50%A；20～30min, 50%A；30～
33min, 50～0%A；33～38min, 100%B；Column temperature：35℃；Flow velocity：1.0mL/min；Sample size：10μL；Detector
The parameter of ELSD：Drift tube temperature is 95 DEG C；Nitrogen flow rate is 2.5mL/min；
Distinguish sample introduction analysis compound sugar mixed sample, multiple pure honey samples and honey sample to be checked with this understanding,
Obtain the chromatographic fingerprinting of the chromatogram and honey sample of mixed sample；Chromatographic retention according to compound sugar mixed sample
Corresponding to monose and different polymerization degree compound sugar in the chromatographic fingerprinting of qualitative pure honey sample and honey sample to be checked
Chromatographic peak, and with the 7th total peak as reference peak, calculate the relative retention time of each fingerprint peakses；
(3) determination of honey chromatographic fingerprint common characteristic peaks
By the HPLC fingerprint analysis of the compound sugar and its isomers of pure honey sample, compare its chromatogram, according to peak
Relative retention time determine 8 common characteristic peaks, be calculated 8 with the 7th common characteristic honeybee as reference by peak sequence
The relative retention time (RT) of common characteristic peaks is as follows：
The average RT in No. 1 peak is 0.24% for 0.767, RSD；
The average RT in No. 2 peaks is 0.41% for 0.806, RSD；
The average RT in No. 3 peaks is 0.22% for 0.852, RSD；
The average RT in No. 4 peaks is 0.13% for 0.885, RSD；
The average RT in No. 5 peaks is 0.13% for 0.916, RSD；
The average RT in No. 6 peaks is 0.09% for 0.954, RSD；
The average RT in No. 7 peaks is 0.00% for 1.000, RSD；
The average RT in No. 8 peaks is 1.44% for 1.118, RSD；
(4) offset minimum binary-discriminant analysis
Total chromatographic peak is integrated, is relative peak face with the peak area at each peak and the ratio of the peak area of reference peak
Product is new variables, carries out discriminant analysis using offset minimum binary-discriminant analysis method, carries out true and false classification to the honey for detecting.
In one embodiment of the invention, pure honey sample is 9 kinds or more than 9 kinds different nectar sources, different sources
33 or more than 33 pure honey samples.
Beneficial effects of the present invention：
Using the advantage of hydrophilic Interaction Chromatography separating oligomeric sugar isomers, to the compound sugar in pure honey and adulterated honey
And its isomers carries out separating analysis, according to the difference at their chromatographic fingerprint peak, using partial least squares discriminant analysis method,
The adulterated honey sample that the adulterated amount of malt syrup is more than 5%, the adulterated amount of HFCS is higher than 10% can be identified, instrument is established
Device more popularizes, be easy to honey enterprise of basic unit and testing agency's popularization and application, and to C4 and C3 plant sugar adulterated is suitable for
HPLC adulteration detection methods.
Description of the drawings
Fig. 1：The HPLC-ELSD finger-prints of the oligomeric saccharic composition of 9 kinds of honey samples.
Fig. 2：Pure acacia honey chromatogram.
Fig. 3：The chromatogram contrast of pure acacia honey and two, three, four, five, six saccharides.
Fig. 4：Pure acacia honey is contrasted with the chromatogram respectively mixed with 10%, the 20%, acacia honey of 30% HFCS, its
In, Fig. 4 (b), Fig. 4 (c) they are the enlarged drawing of the two rectangle frame parts in left and right in Fig. 4 (a) respectively.
Fig. 5：Pure acacia honey and chromatogram contrast respectively mixed with the acacia honey of 5%, 10% malt syrup.
Fig. 6：Principal component scores (the t of pure honey and adulterated honey1/t2) 3D figures；The part difference that two dotted ellipses are irised out
Represent adulterated honey, pure honey.
Fig. 7：Proof diagram replaced by PLS-DA models.
Specific embodiment
With reference to embodiment, the present invention will be further described, and following embodiments are merely to illustrate the present invention rather than to this
The restriction of invention.
Embodiment 1：Honey adulteration based on HILIC-ELSD and partial least squares discriminant analysis method is detected
1st, instrument, sample and reagent
1.1 instrument
1100 series of high efficiency liquid chromatographic systems of Agilent：G1313A automatic samplers, G1311C quaternary pumps, match somebody with somebody
Alltech2000 EISDs, Agilent1100 chromatographic work stations.
1.2 samples and reagent
9 kinds of single flower kind honey：Acacia honey, rape honey, honey of lychee flowers, Mel Jujubae, honey of lungan flowers, Mel, loquat honey, snow fat lotus
Honey, chaste honey, totally 33 samples, are provided by bee-keeping association vice president unit Jiangsu day peak Products Co., Ltd of China.
HFCS (F42), malt syrup are respectively by Shandong Xiang Chijian sources bio tech ltd and Lu Zhou biologies section
Skill Co., Ltd provides.
Acetonitrile, chromatographically pure, (Tedia, USA)；Sucrose, analyzes pure (Chemical Reagent Co., Ltd., Sinopharm Group).
Maltose, maltotriose, maltotetraose, maltopentaose and MALTOHAXAOASE standard items (more than 97%, Japan
Hayashibara Biochemical Laboratories, Inc.).
2nd, sample pre-treatments and the preparation for simulating adulterated honey sample
Using above-mentioned 33 9 kinds different nectar source, different sources pure honey samples, gradient 10%, quality is pressed respectively
Fraction 10% to 30%, adds HFCS to prepare an adulterated honey sample collection, obtains adulterated honey sample 99 (33 × 3
=99)；Select 15 pure honey to press mass fraction 5%, 10% respectively, add malt syrup to prepare an adulterated honey sample
Collection, obtains adulterated honey sample 30；Pure honey sample 33；Thus, the sample sets sum of acquisition is 162 (99+33+
30=162).
Above-mentioned 162 samples of 1g are weighed respectively in 25mL volumetric flasks, distilled water is settled to scale, after fully mixing, taken
1mL crosses 0.45 μm of filter membrane, and filtrate is standby in liquid-phase inlet bottle.
3rd, in honey, the chromatographic fingerprint of oligomeric saccharic composition is analyzed
Chromatographic column is 3.5 μm of 4.6 × 250mm of XBridgeTMAmide；Mobile phase：A (50% acetonitrile)-B (75% second
Nitrile) binary gradient elutes.Gradient program：0～20min, 0～50%A；20～30min, 50%A；30～33min, 50～0%
A；33～38min, 0%A (i.e. 100%B).Column temperature：35℃；Flow velocity：1.0mL/min；Sample size：10μL.Detector (ELSD)
Parameter：Drift tube temperature, 95 DEG C；Nitrogen flow rate, 2.5mL/min.
Distinguish sample introduction analysis compound sugar mixed sample and honey sample with this understanding, obtain mixed sample chromatogram and
The chromatographic fingerprinting of honey sample.In chromatographic fingerprinting according to the qualitative honey sample of the chromatographic retention of mixed sample
Monose and different polymerization degree compound sugar corresponding to chromatographic peak, and on the basis of the 7th total peak, calculate the phase of each fingerprint peakses
To retention time.
Referred to by 9 kinds of different nectar sources, the compound sugar of pure honey sample of 33 different sources and its HPLC of isomers
Line is analyzed, and compares its chromatogram, is determined according to the relative retention time at peak and is obtained 8 common characteristic peaks, its relative standard deviation
RSD is respectively less than 2%；
The average RT in No. 1 peak is 0.24% for 0.767, RSD；
The average RT in No. 2 peaks is 0.41% for 0.806, RSD；
The average RT in No. 3 peaks is 0.22% for 0.852, RSD；
The average RT in No. 4 peaks is 0.13% for 0.885, RSD；
The average RT in No. 5 peaks is 0.13% for 0.916, RSD；
The average RT in No. 6 peaks is 0.09% for 0.954, RSD；
The average RT in No. 7 peaks is 0.00% for 1.000, RSD；
The average RT in No. 8 peaks is 1.44% for 1.118, RSD.
8 total chromatographic peaks are integrated, with the peak area at each peak and the peak area of reference peak (the 7th total peak)
Ratio as relative peak area be used for the metrological data processing of subsequent chemistry.
4th, pure honey and the chromatographic peak feature and difference for simulating adulterated honey
Chromatogram of the accompanying drawing 2 for a true acacia honey.According to knowable to the contrast of Standard for Sugars sample chromatogram figure (such as accompanying drawing 3),
Acacia honey is close to (to the rear) for the chromatographic peak of 10.644min (peak 1) with sucrose appearance time in retention time, and acacia honey is last
The retention time at one peak is the chromatographic peak and maltotriose appearance time close (to the front) of 16.195min (peak 8), therefore acacia
Honey retention time be 10.644min (peak 1), 11.209min (peak 2), 11.869min (peak 3), 12.382min (peak 4),
12.878min (peak 5), 13.464min (peak 6), the chromatographic peak at 14.169min (peak 7) place may be disaccharides and its isomers,
And retention time is probably then trisaccharide for the chromatographic peak of 16.195min (peak 8).By true acacia honey and the fruit Portugal mixed with different proportion
The acacia honey chromatogram of syrup and malt syrup contrasted respectively (accompanying drawing 4 and figure accompanying drawing 5) visible, pure acacia honey with adulterated
The difference of acacia honey is concentrated mainly between 10～15min.Accompanying drawing 4 shows, with the increase of HFCS incorporation, 10～
The chromatogram peak height of 13min is gradually reduced, and the time period is described, based on honey component peak；And the chromatogram peak height of 13～15min with
The increase of HFCS incorporation and increase, this shows the time period with HFCS into based on swarming.Equally, by accompanying drawing 5
It can be seen that, with the increase of malt syrup incorporation, simulate the peak height of the chromatographic peak of the 10～12min and 13～15min of adulterated sample
It is gradually reduced, i.e., in this two time period, also based on honey component peak；And the chromatogram peak height of 12～13min is then with maltose
Starch the few increase of incorporation and increase, also illustrate these chromatographic peaks based on malt syrup and its isomers.
5th, partial least squares discriminant analysis
PLS (SIMCA-P11 softwares) is a kind of multivariate statistical method, collection canonical correlation analysis, principal component point
The basic function of analysis and multiple regression linear analysis is integrated, and can eliminate overlapped chemical information during analysis,
So that analyze data is more accurately and reliably.Randomly select 16 samples composition checking collection, remaining 146 sample is training set, and
PLS-DA model validations are evaluated by coefficient R 2 and cross validation regression coefficient Q2.All chromatograms by sample
The relative peak area at peak carries out statistical analysis as variable.2 principal components are extracted, the accumulation interpretability of independent variable is
48.5%, be 34.8% to the interpretability of dependent variable, in principal component scores figure (as shown in Figure 6), pure honey with mixed with
The honey sample of HFCS does not intersect, and shows that the model can be classified well to sample.
6th, the analysis of PLS-DA models
The set that all of sample is constituted is divided into two classes, the first kind is all of pure honey, and Equations of The Second Kind is all of
Adulterated honey (including HFCS and malt syrup).The permutation test experiment of 20 times is carried out to model, as shown in Figure 7.Knot
Really show, the R of all points positioned at the left side2And Q2Value (Y-axis data) is below the R of rightmost point2And Q2Value, and Q2The tropic
Intercept is respectively less than zero, illustrates that PLS-DA discrimination models do not have the phenomenon of over-fitting, and being determined with preferably to true and false honey
Predictive ability.
7th, PLS-DA models are to sample classification results
By tabulation come the classification capacity of assessment models.To the criterion of each sample it is：1. when Y is more than
0.5, and deviation be less than 0.5 when, judge sample belong to such, 2. when Y be less than 0.5, deviation be less than 0.5 when, judge be not belonging to this
Class, 3. when Y is about 0.5, judges unstable [100], sample segment result of determination such as table 1, wherein the numeral more than 0.5 is used
" overstriking " is marked, and the sample of misjudgement is marked with " overstriking italic ".Differentiation rate through counting in training set is 94.02%, checking collection
Forecasting recognition rate be 100%, therefore, can show that PLS-DA models are preferable to honey adulteration identification result.
1 sample segment classification results list of table
Above test display, the above-mentioned honey adulteration detection side based on HPLC-ELSD and partial least squares discriminant analysis method
Method neither be based on stable carbon isotope rule of three, nor being examined according to characteristic material in a certain plant source syrup
Survey, therefore, its method is adulterated for the starch syrup (including HFCS and malt syrup) in C4 plant sources or C3 plant source
Honey effectively can differentiate, and analytical instrument used is compared with popularization, easy to utilize.
Although the present invention is disclosed as above with preferred embodiment, which is not limited to the present invention, any is familiar with this skill
The people of art, without departing from the spirit and scope of the present invention, can do various changes and modification, therefore protection model of the invention
Enclosing should be by being defined that claims are defined.
Claims (6)
1. a kind of honey adulteration detection method based on HPLC-ELSD and partial least squares discriminant analysis method, it is characterised in that sample
After product are through water-soluble, filtration treatment, pure honey analyzed using the method for hydrophilic Interaction Chromatography separation-Evaporative light scattering detector and is mixed
There are compound sugar and its isomer component in the honey sample of HFCS, malt syrup, and using pure honey and adulterated honey
Oligomeric saccharic composition finger-print difference, carry out data processing and then realizing adulterated mirror by partial least squares discriminant analysis method
Not.
2. method according to claim 1, it is characterised in that comprise the following steps：
1) standard finger-print of different sources, the pure honey compound sugar in different nectar sources and its isomers composition is built first,
Will several different sources, honey sample water dissolves constant volume and the filtration in different nectar source, then efficient liquid phase is carried out to them
Chromatographic isolation and Evaporative light scattering detector, the relative retention time according to gained finger-print determine common characteristic peaks or by gained
Chromatographic data imports finger-print special-purpose software and obtains the compound sugar standard colour chart finger-print of honey and determine its common characteristic
Peak；
2) the compound sugar finger-print for obtaining honey sample to be checked is determined；
3) by step 2) the relative peak area data of the finger-print of honey sample to be checked that obtain and step 1) obtain some
Individual different sources, the relative peak area data composition matrix of the finger-print of the pure honey sample in different nectar sources, are carried out partially most
A young waiter in a wineshop or an inn takes advantage of discriminant analysis.
3. method according to claim 1 and 2, it is characterised in that comprise the following steps：
(1) pretreatment of honey sample to be checked
Sample pretreatment：1-2g honey samples to be checked are weighed in 25mL or 50mL volumetric flasks, distilled water constant volume, shake well are mixed
After even, take 1mL and cross 0.45 μm of miillpore filter, filtrate is used for the HPLC analyses of compound sugar and its isomers；
(2) honey sample to be checked, the liquid-phase chromatographic analysis of compound sugar mixed sample
Chromatographic condition：Chromatographic column is 3.5 μm of 4.6 × 250mm of XBridgeTM Amide；Mobile phase A is 50% acetonitrile, mobile phase
B is 75% acetonitrile, binary gradient elutes, Gradient program：0～20min, 0～50%A；20～30min, 50%A；30～
33min, 50～0%A；33～38min, 100%B；Column temperature：35℃；Flow velocity：1.0mL/min；Sample size：10μL；Detector
The parameter of ELSD：Drift tube temperature is 95 DEG C；Nitrogen flow rate is 2.5mL/min；
Distinguish sample introduction analysis compound sugar mixed sample, multiple pure honey samples and honey sample to be checked with this understanding, obtain
Chromatographic fingerprinting；According to the qualitative pure honey sample of chromatographic retention and honey sample to be checked of compound sugar mixed sample
The chromatographic peak corresponding to monose and different polymerization degree compound sugar in chromatographic fingerprinting, and with the 7th total peak as reference peak,
Calculate the relative retention time of each fingerprint peakses；
(3) determination of honey chromatographic fingerprint common characteristic peaks
By the HPLC fingerprint analysis of the compound sugar and its isomers of pure honey sample, compare its chromatogram, according to the phase at peak
8 common characteristic peaks are determined to retention time, by peak sequence with the 7th common characteristic honeybee as reference, are calculated 8 and are had
The relative retention time of characteristic peak；
(4) offset minimum binary-discriminant analysis
Total chromatographic peak is integrated, is that relative peak area is with the peak area at each peak with the ratio of the peak area of reference peak
New variables, carries out discriminant analysis using offset minimum binary-discriminant analysis method, carries out true and false classification to the honey for detecting.
4. method according to claim 3, it is characterised in that the relative retention time of 8 common characteristic peaks is as follows：
The average RT in No. 1 peak is 0.24% for 0.767, RSD,
The average RT in No. 2 peaks is 0.41% for 0.806, RSD；
The average RT in No. 3 peaks is 0.22% for 0.852, RSD,
The average RT in No. 4 peaks is 0.13% for 0.885, RSD,
The average RT in No. 5 peaks is 0.13% for 0.916, RSD,
The average RT in No. 6 peaks is 0.09% for 0.954, RSD,
The average RT in No. 7 peaks is 0.00% for 1.000, RSD,
The average RT in No. 8 peaks is 1.44% for 1.118, RSD.
5. method according to claim 3, it is characterised in that pure honey sample be 9 kinds or more than 9 kinds different nectar sources,
33 of different sources or more than 33 pure honey samples.
6. according to the arbitrary described method of Claims 1 to 5, it is characterised in that the compound sugar is two to six for the degree of polymerization
Low polymerization sugar, including their isomers.
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| CN107192770A (en) * | 2017-04-24 | 2017-09-22 | 山东省食品药品检验研究院 | A kind of analysis method for differentiating chaste honey and the adulterated chaste honey of syrup |
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