CN102662008A - Method for testing content of lauric acid in coconut food - Google Patents
Method for testing content of lauric acid in coconut food Download PDFInfo
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Abstract
The invention provides a method for testing lauric acid component in coconut milk, coconut powder and other coconut food, which comprises the preparation of a test sample, the preparation of standard working solution and gas chromatography analysis; and the extraction, the methyl esterification and the quantification of lauric acid in the coconut food are completed through the three steps. The method is an objective and effective test means for analyzing the quality of the coconut food, so that the detects of adulteration and low quality which are easy to occur if items for controlling the quality of the coconut food are not too few (physical and chemical control indexes of the current coconut food only comprise two items, i.e. the content of protein and fat) are overcome, and the hidden hazards of food quality safety accidents are avoided.
Description
Technical field
The present invention relates to a kind of detection method, specifically, relate to a kind of detection method coconut based foods such as coconut milk, coconut palm slurry, coconut powders.
Background technology
Food-safety problem has been a very serious problem at present, strengthens detecting, set up perfect food safety detection system, and set up control criterion, and be the effective measures that ensure food safety.For the coconut based food, its quality control project (the physics and chemistry controlling index of coconut based food has only two of protein and fat contents at present) on the low side at present, thus cause the coconut based food to occur mingling, mix low etc. the food quality security incident of puppet, quality easily.Therefore press for and explore a cover lauric extraction in the coconut based food, purifying, quantitative detection method; Set up the lauric acid content standard in the product; In present industry standard, add this controlling index of lauric acid; With this total quality of controlling product, avoid occurring the hidden danger of food quality security incident.
The history in existing more than 2000 year of China's plantation coconut; Mainly concentrate on various places, Hainan Province, coconut occupies an important position in the industrial crops of Hainan, and nutritive value is very high at present; Modern scientific research shows; Contain trace element and mineral matters such as protein, carbohydrate, grease class, vitamins and calcium, phosphorus, iron in Coconut Juice and the coconut meat, development numerous food capable of using in the food industry is like coconut palm fruit, arrack, coconut water drink etc.
The coconut main body of oil is main with lauric acid, contains unsaturated fatty acids such as saturated fatty acids such as caproic acid, sad, capric acid, myristic acid, palmitic acid, stearic acid and a small amount of oleic acid in addition.Lauric acid, promptly dodecylic acid is an important chemical material, mainly is to utilize some natural plant greases to make through technologies such as hydrolysis, rectifying.The lauric content that at present existing bibliographical information utilizes gas chromatography to come the grey seed nucleolus oil in direct and quick determination hydrolysis mountain to make.Also there is document to adopt the GC-FID method that the fatty acid composition in the coconut oil has been carried out analyzing report, also has bibliographical information to use high temperature gas chromatography one EI mass spectrum (GC-MS) method that the fatty acid triglycercide in the coconut oil is analyzed.But at present not bibliographical information to lauric extraction in the coconut based foods such as coconut milk, coconut palm slurry, coconut powder, purifying, quantitative a whole set of detection method.Therefore set up a cover to lauric extraction in the coconut based food, purifying, quantitative detection method; Formation is to the accumulation of a series of detection data of product; Thereby set up the lauric acid content standard in the product; In present industry standard, add this controlling index of lauric acid, significant with this total quality of controlling the coconut based food.
Summary of the invention
The purpose of this invention is to provide a kind of detection method to coconut based foods such as coconut milk, coconut palm slurry, coconut powders; Be used to improve the quality control level of coconut based food; This method is a kind of objective detection means that effectively is used to analyze coconut based food quality; Thereby avoid coconut based food quality control project (at present the physics and chemistry controlling index of coconut based food has only two of protein and fat contents) on the low side; Occur mixing puppet, low-quality defective easily, avoid occurring the hidden danger of food quality security incident.
Technical scheme of the present invention: utilize and to set up a cover to lauric extraction in the coconut based food, purifying, quantitative detection method; Formation is to the accumulation of a series of detection data of product; Thereby set up the lauric acid content standard in the product; In present industry standard, add this controlling index of lauric acid, control the total quality of product with this.
The detection method that the present invention relates to lauric acid content in the coconut based food, step is following:
Step 1: setup test sample: comprise and extract fat and saponification, the lauric acid in the specimen is converted into methyl laurate;
Step 2: the preparation of standard operation liquid: comprise the preparation of lauric acid standard stock solution and the preparation of methyl laurate standard operation liquid;
Step 3: gas chromatographic analysis analyzing and processing: treat the spectrogram of the titer of sample measuring liquid and preparation through analysis, obtain lauric content in the coconut based food.
Accomplish lauric extraction in the coconut based food, esterification, quantitative detection method through above-mentioned steps.
Because lauric acid is the characteristic chemical constituent of coconut, belongs to saturated fatty acid, boiling point is 299 ℃, and from the consideration of safety and testing conditions, the methyl laurate that is translated into boiling point lower (261～262 ℃) among the present invention carries out detection by quantitative.
This detection method is in the step of extracting fat; For testing sample is the fat-extraction of coconut palm slurry or coconut milk, mainly is at the colloid proterties and the fat globule membrane that add ammoniacal liquor, ethanolic solution destruction breast, makes fat dissociate out; Add sherwood oil, ether again, extract crude fat.
Fat-extraction for coconut powder then adopts traditional soxhlet extraction, then to the methanol solution saponification with NaOH of the fatty acid that extracts, lets saponified again and BF3-ether mixed solution reaction conversion is a fatty acid methyl ester, obtains treating sample measuring liquid.Treat the spectrogram of the titer of sample measuring liquid and preparation at last through gas chromatographic analysis, obtain lauric content in the coconut based food.
The detection method to lauric acid content in the coconut based food that the present invention relates to is specific as follows:
Step 1, setup test sample
Comprise and extract fat and saponification that the lauric acid in the specimen is converted into methyl laurate, and concrete steps are following:
(1) extracts fatty step
A, be the fat-extraction of coconut palm slurry or coconut milk: draw 10.0ml coconut milk or 2～5g coconut palm slurry sample in the 100ml graduated cylinder, add 1.25ml ammoniacal liquor, fully mixing for testing sample; Put in 60 ℃ of water-baths and heat 15min; Jolting 2min adds 10ml ethanol, fully shakes up; In cold water, after the cooling, add the 10ml ether, jolting 0.5min adds the 10ml sherwood oil, and jolting 0.5min leaves standstill 30min, when treating the upper strata clarification, reads organic layer volume and record; In round-bottomed flask, ether is flung in water-bath to absorption organic layer extract 10.0ml, gets residue in 50ml;
B, be the fat-extraction of coconut powder: take by weighing 2～5g coconut powder sample, move in the filtration paper cylinder for testing sample; Filtration paper cylinder is put into the extracting tube of fatty extractor, connects dry 100ml round-bottomed flask, add 2/3rds places of absolute ether, in water-bath, heat to the bottle inner volume, make the continuous refluxing extraction of ether (6 times/h-8 time/h), general extracting 6h-12h; After extracting completion, withdrawing device is transferred to the ether extracted liquid in the receiving bottle in the 50ml volumetric flask, is settled to scale.In round-bottomed flask, ether is flung in water-bath to absorption 20.0ml extract, gets residue in 50ml;
(2) saponification step: the residue in the step (1) is dissolved with normal hexane; Normal hexane consumption 3～8mL; The sodium hydrate methanol solution that adds 3～8mL again; Connect condenser, the 12-18min that in the water-bath of preference temperature, refluxes adds 3～8m L boron trifluoride-ether from condenser overhead again and continues backflow 3min; Stop heating, the related condensing unit of flask is taken out from firing equipment, add the 5ml normal hexane immediately from the condenser pipe top, be cooled to room temperature; Take off flask, add 12～18ml saturated nacl aqueous solution, filled in bottle stopper, acutely shake 15s at least; Continue to add saturated nacl aqueous solution to the flask neck place, standing demix is transferred to the upper strata n-hexane extract in the 25ml volumetric flask with dropper, repeatedly extracts with normal hexane again; Be settled to scale, shake up, for treating sample measuring liquid; This saponification step promptly is that lauric acid changes methyl laurate into.
The preparation of step 2, standard operation liquid:
Comprise the preparation of lauric acid standard stock solution and the preparation of methyl laurate standard operation liquid; Concrete steps are following:
(1) preparation of lauric acid standard stock solution: take by weighing lauric acid standard items 0.6g in the brown volumetric flask of 50mL,, shake up, be stored in the refrigerator subsequent use with normal hexane dissolving and constant volume;
(2) preparation of methyl laurate standard operation liquid: pipette lauric acid standard stock solution 5.0mL; The sodium hydrate methanol solution that adds 3～8mL; Connect condenser, the 12-18min that in the water-bath of preference temperature, refluxes adds 3～8mL boron trifluoride-ether from condenser overhead again and continues backflow 3min; Stop heating, the related condensing unit of flask is taken out from firing equipment, add the 5ml normal hexane immediately from the condenser pipe top, be cooled to room temperature; Take off flask, add 12～18ml saturated nacl aqueous solution, filled in bottle stopper, acutely shake 15s at least; Continue to add saturated nacl aqueous solution to the flask neck place, standing demix is transferred to the upper strata n-hexane extract in the 25ml volumetric flask with dropper, repeatedly extracts with normal hexane again; Be settled to scale, shake up, be methyl esters standard solution (promptly obtaining the standard reserving solution of esterification after the above-mentioned steps); Standard reserving solution after the esterification is transferred in the 25ml volumetric flask, is settled to scale, shake up with normal hexane.Draw above-mentioned solution 0.5,1.0,2.0,3.0,4.0 respectively in the 5ml volumetric flask, be settled to scale, shake up, be methyl laurate standard operation solution;
Step 3, gas chromatographic analysis:
Treat the spectrogram of the titer of sample measuring liquid and preparation through analysis, obtain lauric content in the coconut based food; Specific analytical method is following:
The reference conditions of gas chromatography: chromatographic column: Agilent HP-5 capillary column 30m * 0.25mm * 0.25 μ m; Flow rate of carrier gas: 1.0ml/min (constant current mode); Heating schedule: 150 ℃ of initial temperatures, rise to 250 ℃ with 10 ℃/min, keep 3min; 250 ℃ of injector temperatures; Detector temperature: 280 ℃; Split sampling (split ratio): 50: 1, sample size: 1 μ l; Flow velocity: nitrogen 40ml/min; Hydrogen 40ml/min; Air 400ml/min;
With the methyl laurate standard operation liquid sample introduction under above-mentioned chromatographic condition for preparing in the step 2, qualitative with retention time, chromatographic peak area is quantitative.With lauric acid concentration (mg/ml) is horizontal ordinate, is that ordinate is formulated typical curve with the peak area integration; With treating sample measuring liquid sample introduction under above-mentioned chromatographic condition under the steps A (2), quantitative with the chromatographic peak area integration.
Lauric content is by calculating as shown in the formula (1) in the sample:
In the formula:
X---lauric content (g/100g) in the sample
A
1---the peak area of methyl laurate in the sample solution
A
2---the peak area of methyl laurate in the lauric acid acid methyl esters standard operation liquid
The concentration (mg/mL) of C---methyl laurate standard operation liquid
The sampling amount of M---sample (g)
M1---lauric molecular mass
The molecular mass of M2---methyl laurate
P---the volume fraction of sample sampling
V---the constant volume of n-hexane extract after the sample esterification.
The result keeps a decimal, and the independent result's of mensuration of twice of under repeated condition, obtaining absolute difference must not surpass 10% of mean value.
Method of the present invention can be measured the lauric acid content in the existing in the market coconut series products, for the quality of controlling this series products provides foundation.
Description of drawings
Fig. 1. the drafting of typical curve (gas chromatogram of the methyl laurate standard operation liquid of C=1.0722mg/mL);
Fig. 2. the drafting of typical curve (gas chromatogram of the methyl laurate standard operation liquid of C=2.1444mg/mL).
Fig. 3. coconut milk sample analysis gas chromatogram (lot number: 20110925);
Fig. 4. coconut milk sample analysis gas chromatogram (lot number: 20111113);
Embodiment one
1. (get every jar of original flavor coconut milk of 245ml/ sample of coconut palm island, Hainan Group Plc production of two lot numbers: the extraction of fat 20110925 and 20111113): absorption 10.0ml coconut milk sample adds 1.25ml ammoniacal liquor, abundant mixing to the coconut milk sample in 100ml tool plug graduated cylinder; Put in 60 ℃ of water-baths and heat 15min, jolting 2min adds 10ml ethanol; Fully shake up, in cold water, after the cooling, add the 10ml ether; Jolting 0.5min adds the 10ml sherwood oil, jolting 0.5min; Leave standstill 30min, when treating the upper strata clarification, read ether layer volume and record.
2. saponification: draw step 1 extract 10.0ml down in 50ml in round-bottomed flask, ether is flung in water-bath, must residue.Residue is used the 5ml n-hexane dissolution, add the 5ml sodium hydrate methanol solution, connect condenser, the 15min that in 70 ℃ of water-baths, refluxes adds 5ml boron trifluoride-ether from condenser overhead again and continues backflow 3min.Stop heating, the related condensing unit of flask is taken out from firing equipment, add the 5ml normal hexane immediately from the condenser pipe top, be cooled to room temperature; Take off flask, add about 15ml saturated nacl aqueous solution, filled in bottle stopper, acutely shake 15s at least; Continue to add saturated nacl aqueous solution to the flask neck place, standing demix is transferred to the upper strata n-hexane extract in the 25ml volumetric flask with dropper, repeatedly extracts with normal hexane again; Be settled to scale, shake up, for treating sample measuring liquid.
3. typical curve preparation:
(1) preparation of lauric acid standard reserving solution: accurately take by weighing lauric acid standard items 0.67g (being accurate to 0.0001) in the brown capacity of 50ml,, shake up, be stored in the freezer compartment of refrigerator subsequent use with n-hexane dissolution and constant volume.
(2) preparation of methyl laurate standard operation liquid: accurately draw 5.0ml lauric acid standard reserving solution; 2 are risen from " adding the 5ml sodium hydrate methanol solution ... " down and carry out esterification and handle set by step; Standard reserving solution after the esterification is transferred in the 25ml volumetric flask; Be settled to scale with normal hexane, shake up.Draw above-mentioned solution 0.5,1.0,2.0,3.0,4.0 respectively in the 5ml volumetric flask, be settled to scale, shake up.
(3) reference conditions of gas chromatography: chromatographic column: HP-FFAP, 30m * 0.25mm, 0.25 μ m; Carrier gas: high pure nitrogen; Injector temperature: 250 ℃; Detector temperature: 280 ℃; The column oven temperature: 150 ℃ of initial temperatures, be raised to 250 ℃ with 10 ℃/min, keep 3min; Flow rate of carrier gas: 1.0mL/min.
(4) preparation of typical curve: chromatographic condition sample introduction in (3) set by step, interpretation of result, utilization instrument workstation production standard curve, and be saved in the Instrument measuring method.(result is as shown in table 1, and spectrogram is seen Fig. 1 and Fig. 2).(r＞0.995)
4. sample determination:
(1) with treating sample measuring liquid chromatographic condition sample introduction in (3) set by step after the esterification, does parallel appearance (spectrogram is seen Fig. 3 and Fig. 4) simultaneously.
(2) result calculates:
In the formula:
X---lauric content (g/100g) in the sample
A
1---the peak area of methyl laurate in the sample solution
A
2---the peak area of methyl laurate in the lauric acid acid methyl esters standard operation liquid
The concentration (mg/mL) of C---methyl laurate standard operation liquid
The sampling amount of M---sample (g)
M
1---lauric molecular mass
M
2---the molecular mass of methyl laurate
P---the volume fraction of sample sampling
V---the constant volume of n-hexane extract after the sample esterification.
The result keeps a decimal, and the independent result's of mensuration of twice of under repeated condition, obtaining absolute difference must not surpass 10% of mean value.
The drafting of table 1 typical curve
Table 2 sample analysis result
A kind of detection method to lauric acid content in the coconut based food of the present invention is described through concrete embodiment.Those skilled in the art can use for reference links such as content appropriate change raw material of the present invention, process conditions and realize corresponding other purpose; Its relevant change does not all break away from content of the present invention; All similar replacements and change will become apparent to those skilled in the art that all to be regarded as and are included within the scope of the present invention.
Claims (4)
1.-and kind of detection method to lauric acid content in the coconut based food, step is following:
Step 1: setup test sample: comprise and extract fat and saponification, the lauric acid in the specimen is converted into methyl laurate;
Step 2: the preparation of standard operation liquid: comprise the preparation of lauric acid standard stock solution and the preparation of methyl laurate standard operation liquid;
Step 3: gas chromatographic analysis analyzing and processing: treat the spectrogram of the titer of sample measuring liquid and preparation through analysis, obtain lauric content in the coconut based food.
2. according to the detection method of claim 1, wherein the concrete steps of the related setup test sample of step 1 are following:
(1) extracts fatty step
A, be the fat-extraction of coconut palm slurry or coconut milk: draw 10.0ml coconut milk or 2～5g coconut palm slurry sample in the 100ml graduated cylinder, add 1.25ml ammoniacal liquor, fully mixing for testing sample; Put in 60 ℃ of water-baths and heat 15min; Jolting 2min adds 10ml ethanol, fully shakes up; In cold water, after the cooling, add the 10ml ether, jolting 0.5min adds the 10ml sherwood oil, and jolting 0.5min leaves standstill 30min, when treating the upper strata clarification, reads organic layer volume and record; In round-bottomed flask, ether is flung in water-bath to absorption organic layer extract 10.0ml, gets residue in 50ml;
B, be the fat-extraction of coconut powder: take by weighing 2～5g coconut powder sample, move in the filtration paper cylinder for testing sample; Filtration paper cylinder is put into the extracting tube of fatty extractor, connects dry 100ml round-bottomed flask, add 2/3rds places of absolute ether, in water-bath, heat to the bottle inner volume, make the continuous refluxing extraction of ether (6 times/h-8 time/h), general extracting 6h-12h; After extracting completion, withdrawing device is transferred to the ether extracted liquid in the receiving bottle in the 50ml volumetric flask, is settled to scale.In round-bottomed flask, ether is flung in water-bath to absorption 20.0ml extract, gets residue in 50ml;
(2) saponification step: the residue in the step (1) is dissolved with normal hexane; Normal hexane consumption 3～8mL; The sodium hydrate methanol solution that adds 3～8mL again; Connect condenser, the 12-18min that in the water-bath of preference temperature, refluxes adds 3～8m L boron trifluoride-ether from condenser overhead again and continues backflow 3min; Stop heating, the related condensing unit of flask is taken out from firing equipment, add the 5ml normal hexane immediately from the condenser pipe top, be cooled to room temperature; Take off flask, add 12～18ml saturated nacl aqueous solution, filled in bottle stopper, acutely shake 15s at least; Continue to add saturated nacl aqueous solution to the flask neck place, standing demix is transferred to the upper strata n-hexane extract in the 25ml volumetric flask with dropper, repeatedly extracts with normal hexane again; Be settled to scale, shake up, for treating sample measuring liquid.
3. according to the detection method of claim 1, wherein the preparation concrete steps of the related standard operation liquid of step 2 are following:
(1) preparation of lauric acid standard stock solution: take by weighing lauric acid standard items 0.6g in the brown volumetric flask of 50mL,, shake up, be stored in the refrigerator subsequent use with normal hexane dissolving and constant volume;
(2) preparation of methyl laurate standard operation liquid: pipette lauric acid standard stock solution 5.0mL; The sodium hydrate methanol solution that adds 3～8mL; Connect condenser, the 12-18min that in the water-bath of preference temperature, refluxes adds 3～8mL boron trifluoride-ether from condenser overhead again and continues backflow 3min; Stop heating, the related condensing unit of flask is taken out from firing equipment, add the 5ml normal hexane immediately from the condenser pipe top, be cooled to room temperature; Take off flask, add 12～18ml saturated nacl aqueous solution, filled in bottle stopper; Acutely shake 15s at least, continue to add saturated nacl aqueous solution to flask neck place, standing demix; Standard reserving solution after the esterification is transferred in the 25ml volumetric flask, is settled to scale, shake up with normal hexane.Draw above-mentioned solution 0.5,1.0,2.0,3.0,4.0 respectively in the 5ml volumetric flask, be settled to scale, shake up, be methyl laurate standard operation solution.
4. according to the detection method of claim 1, wherein the related gas chromatographic analysis analyzing and processing of step 3 is specific as follows:
The reference conditions of gas chromatography: chromatographic column: Agilent HP-5 capillary column 30m * 0.25mm * 0.25 μ m; Flow rate of carrier gas: 1.0ml/min (constant current mode); Heating schedule: 150 ℃ of initial temperatures, rise to 250 ℃ with 10 ℃/min, keep 3min; 250 ℃ of injector temperatures; Detector temperature: 280 ℃; Split sampling (split ratio): 50: 1, sample size: 1 μ l; Flow velocity: nitrogen 40ml/min; Hydrogen 40ml/min; Air 400ml/min;
With the methyl laurate standard operation liquid sample introduction under above-mentioned chromatographic condition for preparing in the step 2, qualitative with retention time, chromatographic peak area is quantitative.With lauric acid concentration (mg/ml) is horizontal ordinate, is that ordinate is formulated typical curve with the peak area integration; With treating sample measuring liquid sample introduction under above-mentioned chromatographic condition under the steps A (2), quantitative with the chromatographic peak area integration.
Lauric content is by calculating as shown in the formula (1) in the sample:
In the formula:
X---lauric content (g/100g) in the sample
A
1---the peak area of methyl laurate in the sample solution
A
2---the peak area of methyl laurate in the lauric acid acid methyl esters standard operation liquid
The concentration (mg/mL) of C---methyl laurate standard operation liquid
The sampling amount of M---sample (g)
M
1---lauric molecular mass
M
2---the molecular mass of methyl laurate
P---the volume fraction of sample sampling
V---the constant volume of n-hexane extract after the sample esterification.
The result keeps a decimal, and the independent result's of mensuration of twice of under repeated condition, obtaining absolute difference must not surpass 10% of mean value.
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Cited By (1)
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| CN105823760A (en) * | 2016-03-11 | 2016-08-03 | 无锡初晨生物科技有限公司 | Method for evaluating coconut quality |
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| EP1188442A2 (en) * | 2000-09-13 | 2002-03-20 | Wei Xiao | Cinnamomi and poria composition, method to prepare the same and uses thereof |
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2012
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1188442A2 (en) * | 2000-09-13 | 2002-03-20 | Wei Xiao | Cinnamomi and poria composition, method to prepare the same and uses thereof |
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| CN105823760A (en) * | 2016-03-11 | 2016-08-03 | 无锡初晨生物科技有限公司 | Method for evaluating coconut quality |
| CN105823760B (en) * | 2016-03-11 | 2018-09-25 | 无锡初晨生物科技有限公司 | A kind of method for evaluating quality of coconut palm fruit |
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Application publication date: 20120912 |