CN1776429A - Apple raw juice identifying method - Google Patents

Apple raw juice identifying method Download PDF

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Publication number
CN1776429A
CN1776429A CN 200510126179 CN200510126179A CN1776429A CN 1776429 A CN1776429 A CN 1776429A CN 200510126179 CN200510126179 CN 200510126179 CN 200510126179 A CN200510126179 A CN 200510126179A CN 1776429 A CN1776429 A CN 1776429A
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sample
malic acid
acid
utilize
juice
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CN100559184C (en
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胡小松
高海燕
吴继红
廖小军
陈芳
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China Agricultural University
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China Agricultural University
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Abstract

The method includes steps: (1) detecting D - malic acid; (2) measuring parameter index and calculating content of malic acid. Mathematic model of character of apple natural juice is a creative application made by the invention. Measuring each parameter index accomplishes measurement for malic acid in sample. The model eliminates influences from each environmental factor, possessing systematicality and all sidedness. Comparing current method, the invention overcomes limitation, inaccuracy and difficult operability and possesses advantages of simple testing method and no need of costly instrument.

Description

A kind of method of differentiating apple fumet
Technical field
The present invention relates to differentiate the method for apple fumet.
Background technology
Fruit juice is the elite of fruit, is rich in multiple nutritional components, and color and luster is vivid, and is tasteful, extremely consumer's favor.Along with the raising day by day of living standards of the people and the continuous variation of demand, people replace the beverage of various synthetic gradually with fruit juice and beverage thereof, the consumption figure of fruit juice class beverage is more and more big, yet because the restriction of fruit raw material and productive capacity, the production cost of fruit juice is higher, impel some dishonest manufacturers in pure juice, to add cheap fruit juice thus or fill with the synthetic material fully and cook fruit drink, obtain profit with this, according to statistics, there is the fruit juice of 50-80% being mingled in varying degrees in the world.In Dec, 2003, what State Industry ﹠ Commerce Administration announced shows that to the up-to-date sampling result of fruit juice overall qualification rate is 55%, and wherein the underproof reason of product mainly is that juice content and label are defective.
Cider is the principal item of fruit drink, and China is apple production big country, cider big export country especially, in recent years, the concentrated apple juice development rapidly, the cider industrial market potentiality of China are very huge.Because cider is a kind of multi-component mixed system, proterties is subjected to the influence of many factors again, and therefore, mingling of cider is easy to take place, and mingles a large amount of existence of fruit juice, severe impairment consumer's interests and health.Therefore in order to safeguard consumer's interests, guarantee the import and export quality of this series products, promote the development of cider industry, seek a kind of science and practical, simple and the accurate true and false detection method of cider is extremely urgent.
At present the true and false detection method of cider of report has: particular instrument analytic approach and standard model relative methods such as special component discriminance such as carbohydrate, organic acid, phenols, inorganic elements, amino acid and stable isotope, spectroscopic methodology, location specific natural isotopic classification-nuclear magnetic resonance method, these methods are the routine analyzer complexity not only, length consuming time, the expense height, and need be undertaken by the analysis Instrument equipment of costliness, some is difficult to finish in ordinary laboratory; Simultaneously because the fruit juice ingredient is a lot, the kind of its ingredient and quantity change with the variation of factors such as kind, the place of production, weather, the methods of cultivation, time, fertilizer, agricultural chemicals, and existing these methods are not considered the influence of these factors, lack certain systematicness and integrality, have limitation separately on using, misjudgment phenomenon appears in result easily sometimes.
Summary of the invention
The true and false method of evaluation apple fumet that the purpose of this invention is to provide a kind of easy, strong operability.
The method of discriminating apple fumet provided by the present invention comprises the steps:
1) content of working sample D-malic acid, if having the D-malic acid in the sample, then interpret sample is a doping fruit juice; If do not have the D-malic acid in the sample, then carried out for second step;
2) utilize total acid number X in the determination of acid-basetitration sample 1, in g/100ml, and 0.15g/100mL≤X 1
Utilize 3,5 dinitrosalicylic acid colorimetric method for determining total reducing sugar values, obtain total reducing sugar value/total acid number X 2, and 9.60≤X 2≤ 99.14;
Utilize fructose X in the HPLC method working sample 3With glucose X 4, and 3.34g/100ml≤X 3≤ 7.93g/100ml, 0.33≤X 4≤ 0.88;
Utilize coumaric acid X in the HPLC method working sample 5, in mg/L;
Measure buffer capacity X 6: with 0.1mol/L NaOH titration samples of juice, measure the pH value, press the volume calculation buffer capacity X that 100ml fruit juice changes 1 used NaOH of pH unit with pH meter 6, in ml, and 13ml≤X 6≤ 50.60ml;
Then, according to L MALIC ACID Y in the formula I calculation sample, in mg/L;
Y=12.41+38.76X 1-40.74X 4-2.69X 5-294.27X 1 2+ 35.36X 4 2+ 0.25X 5 2-0.089X 6 2-1.82X 1* X 2-9.97X 1* X 6-0.026X 2* X 3+ 0.0127X 2* X 5+ 0.029X 2* X 6+ 2.13X 3* X 4-0.042X 3* X 5-0.358X 4* X 6(formula I)
Adopt L MALIC ACID value Y in the HPLC working sample A, in mg/ml, and 1.67mg/mL≤Y A
If Y A=Y ± 0.20 illustrates that then this sample is an apple fumet; Otherwise, be doping fruit juice.
The mathematical model of apple fumet feature is represented in the application of the invention, finishes mensuration to malic acid in the sample by measuring various parameters, has got rid of various Effect of Environmental, has systematicness and comprehensive; The detection indication test method is simple, need not can finish in general laboratory by more expensive instrument; Method is accurate, rapid, easy operating, has overcome shortcomings such as existing methods limitation, inaccuracy and difficult operability.
Embodiment
Embodiment 1, method validation
1). self-control apple fumet sample, be placed in 4 ℃ of refrigerators to be measured standbyly, utilize the D-malic acid content in the HPLC method assay determination sample to be 0mg/L, promptly in testing sample, do not detect the D-malic acid, continue step 2 operation.
2). utilize the malic acid content in the HPLC method assay determination sample to be 3.08mg/mL, promptly L MALIC ACID content is 3.08mg/mL in the sample, Y A〉=1.67mg/mL;
Utilize the total acid (X in the determination of acid-basetitration sample 1) be 0.276g/100mL, X 1〉=0.15g/100mL;
Utilize the total reducing sugar in 3, the 5 dinitrosalicylic acid colorimetric method for determining samples, obtain total reducing sugar/total acid (X 2) be 36.59,9.60≤X 2≤ 99.14;
Utilize the fructose (X in the HPLC method working sample 3) and glucose (X 4), obtain fructose (X 3) be 5.31g/100mL, glucose (X 4) be 0.60,3.34g/100mL≤X 3≤ 7.93g/100mL, 0.33≤X 4≤ 0.88;
Utilize the coumaric acid (X in the HPLC method working sample 5) be 2.94 (mg/L);
Accurately pipette samples of juice 50ml to be measured,, measure the pH value, obtain buffer capacity (X with pH meter with 0.1mol/L NaOH titration 6) be 22.76mL, 13mL≤X 6≤ 50.60mL continues step 3 operation.
3). the above survey respectively is worth in the substitution binomial model:
Y=12.41+38.76X 1-40.74X 4-2.69X 5-294.27X 1 2+35.36X 4 2+0.25X 5 2-0.089X 6 2-1.82X 1*X 2+9.97X 1*X 6-0.026X 2*X 3+0.0127X 2*X 5+0.029X 2*X 6+2.13X 3*X 4-0.042X 3*X 5-0358X 4*X 6
Calculate Y=3.06mg/mL, because Y A=3.08mg/mL satisfies Y A=Y ± 0.20 condition proves that testing sample is an apple fumet, and the accuracy and the reliability of the inventive method has been described.
The true and false evaluation of embodiment 2 " Huiyuan's 100% cider "
1) gets commercially available " Huiyuan's 100% cider " 500mL and place 4 ℃ of refrigerators to be measured standby, utilize the D-malic acid content in the HPLC method assay determination sample to be 0mg/L, promptly in testing sample, do not detect the D-malic acid, continue step 2 operation.
2) utilize the malic acid content in the HPLC method assay determination sample to be 3.41mg/mL, promptly L MALIC ACID content is 3.44mg/mL in the sample, Y A〉=1.67mg/mL;
Utilize the total acid (X in the determination of acid-basetitration sample 1) be 0.34g/100mL, X 1〉=0.15g/100mL;
Utilize the total reducing sugar in 3, the 5 dinitrosalicylic acid colorimetric method for determining samples, obtain total reducing sugar/total acid (X 2) be 27.66,9.60≤X 2≤ 99.14;
Utilize the fructose (X in the HPLC method working sample 3) and glucose (X 4), obtain fructose (X 3) be 6.57g/100mL, glucose (X 4) be 0.52,3.34g/100mL≤X 3≤ 7.93g/100mL, 0.33≤X 4≤ 0.88;
Utilize the coumaric acid (X in the HPLC method working sample 5) be 0.00 (mg/L);
Accurately pipette samples of juice 50ml to be measured,, measure the pH value, obtain buffer capacity (X with pH meter with 0.1mol/L NaOH titration 6) be 13.70mL, 13mL≤X 6≤ 50.60mL continues step 3 operation.
3). the above survey respectively is worth in the substitution binomial model:
Y=12.41+38.76X 1-40.74X 4-2.69X 5-294.27X 1 2+35.36X 4 2+0.25X 5 2-0.089X 6 2-1.82X 1*X 2+9.97X 1*X 6-0.026X 2*X 3+0.0127X 2*X 5+0.029X 2*X 6+2.13X 3*X 4-0.042X 3*X 5-0.358X 4*X 6
Calculate Y=3.41mg/mL, because Y A=3.44mg/mL satisfies Y A=Y ± 0.20 condition, decidable " Huiyuan's 100% cider " is an apple fumet.
The true and false evaluation of embodiment 3 " big lake 100% cider "
1). get commercially available " big lake 100% cider " 600mL and place 4 ℃ of refrigerators to be measured standby, utilize the D-malic acid content in the HPLC method assay determination sample to be 0mg/L, promptly in testing sample, do not detect the D-malic acid, continue step 2 operation.
2). utilize the malic acid content in the HPLC method assay determination sample to be 5.11mg/mL, promptly L MALIC ACID content is 5.11mg/mL in the sample, Y A〉=1.67mg/mL;
Utilize the total acid (X in the determination of acid-basetitration sample 1) be 0.50g/100mL, X 1〉=0.15g/100mL;
Utilize the total reducing sugar in 3, the 5 dinitrosalicylic acid colorimetric method for determining samples, obtain total reducing sugar/total acid (X 2) be 21.00,9.60≤X 2≤ 99.14;
Utilize the fructose (X in the HPLC method working sample 3) and glucose (X 4), obtain fructose (X 3) be 8.06g/100mL, glucose (X 4) be 0.80,3.34g/100mL≤X 3≤ 7.93g/100mL, 0.33≤X 4≤ 0.88;
Utilize the coumaric acid (X in the HPLC method working sample 5) be 2.24 (mg/L);
Accurately pipette samples of juice 50ml to be measured,, measure the pH value, obtain buffer capacity (X with pH meter with 0.1mol/L NaOH titration 6) be 20.80mL, 13mL≤X 6≤ 50.60mL continues step 3 operation.
3). the above survey respectively is worth in the substitution binomial model:
Y=12.41+38.76X 1-40.74X 4-2.69X 5-294.27X 1 2+35.36X 4 2+0.25X 5 2-0.089X 6 2-1.82X 1*X 2+9.97X 1*X 6-0.026X 2*X 3+0.0127X 2*X 5+0.029X 2*X 6+2.13X 3*X 4-0.042X 3*X 5-0.358X 4*X 6
Calculate Y=5.21mg/mL, because Y A=5.11mg/mL satisfies Y A=Y ± 0.20 condition, decidable " big lake 100% cider " is an apple fumet.
Whether embodiment 4 " the 5th season " apple juice the evaluation of 100% apple fumet
Get commercially available " the 5th season " apple juice sample 600mL, utilize the D-malic acid content in the HPLC method assay determination sample to be 1579mg/L, in testing sample, detected the existence of D-malic acid, the non-100% real apple fumet of this sample is described, be apple juice, need not to carry out subsequent operation.

Claims (1)

1, a kind of method of differentiating apple fumet comprises the steps:
1) content of working sample D-malic acid, if having the D-malic acid in the sample, then interpret sample is a doping fruit juice; If do not have the D-malic acid in the sample, then carried out for second step;
2) utilize total acid number X in the determination of acid-basetitration sample 1, in g/100ml, and 0.15g/100mL≤X 1
Utilize 3,5 dinitrosalicylic acid colorimetric method for determining total reducing sugar values, obtain total reducing sugar value/total acid number X 2, and 9.60≤X 2≤ 99.14;
Utilize fructose X in the HPLC method working sample 3With glucose X 4, and 3.34g/100ml≤X 3≤ 7.93g/100ml, 0.33≤X 4≤ 0.88;
Utilize coumaric acid X in the HPLC method working sample 5, in mg/L;
Measure buffer capacity X 6: with 0.1mol/L NaOH titration samples of juice, measure the pH value, press the volume calculation buffer capacity X that 100ml fruit juice changes 1 used NaOH of pH unit with pH meter 6, in ml, and 13ml≤X 6≤ 50.60ml;
Then, according to L MALIC ACID Y in the formula I calculation sample, in mg/L;
Y=12.41+38.76X 1-40.74X 4-2.69X 5-294.27X 1 2+ 35.36X 4 2+ 0.25X 5 2-0.089X 6 2-1.82X 1* X 2+ 9.97X 1* X 6-0.026X 2* X 3+ 0.0127X 2* X 5+ 0.029X 2* X 6+ 2.13X 3* X 4-0.042X 3* X 5-0.358X 4X 6(formula I)
Adopt L MALIC ACID value Y in the HPLC working sample A, in mg/ml, and 1.67mg/mL≤Y A
If Y A=Y ± 0.20, then this sample is an apple fumet; Otherwise, be doping fruit juice.
CNB2005101261796A 2005-12-01 2005-12-01 A kind of method of differentiating apple fumet Expired - Fee Related CN100559184C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101929951B (en) * 2009-06-19 2012-06-27 西北农林科技大学 Method for distinguishing milk doped with ewe's milk by near infrared spectrum
CN104215731A (en) * 2014-09-18 2014-12-17 祝伟霞 Method for distinguishing true apple juice from false apple juice by virtue of liquid chromatogram-isotope ratio mass spectrometry (LC-IRMS) determination
CN105067786A (en) * 2014-11-03 2015-11-18 中国食品发酵工业研究院 Identification method of NFC (not from concentration) juice

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101929951B (en) * 2009-06-19 2012-06-27 西北农林科技大学 Method for distinguishing milk doped with ewe's milk by near infrared spectrum
CN104215731A (en) * 2014-09-18 2014-12-17 祝伟霞 Method for distinguishing true apple juice from false apple juice by virtue of liquid chromatogram-isotope ratio mass spectrometry (LC-IRMS) determination
CN105067786A (en) * 2014-11-03 2015-11-18 中国食品发酵工业研究院 Identification method of NFC (not from concentration) juice
CN105067786B (en) * 2014-11-03 2018-02-06 中国食品发酵工业研究院 A kind of discrimination method of non-regenerative fruit juice

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