CN106404971A - Method for identifying rice processing precision by gas chromatography - Google Patents
Method for identifying rice processing precision by gas chromatography Download PDFInfo
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- CN106404971A CN106404971A CN201611071158.3A CN201611071158A CN106404971A CN 106404971 A CN106404971 A CN 106404971A CN 201611071158 A CN201611071158 A CN 201611071158A CN 106404971 A CN106404971 A CN 106404971A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
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- G01N30/8634—Peak quality criteria
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Abstract
The invention provides a method for identifying rice processing precision by gas chromatography, comprising: using an organic solvent to extract a rice sample to obtain extract that includes fats including fatty acid, monoacylglycerol, diacylglycerol and triacylglycerol; subjecting the extract to gas chromatographic analysis to obtain mass percentages of the fats in the rice; acquiring processing precision of the rice sample according to the mass percentages of the fats in the rice and a predetermined standard equation, wherein the standard equation is an equation using the mass percentages of the fats in the rice as independent variables and rice level as a dependent variable, and evaluating the rice processing precision with the rice level. The quantitative relationship of the mass contents of fats in rice to rice level is established herein, rice processing precision is identified by measuring the fat contents in rice, and the method is accurate, simple to perform and low in time consumption and is easy to popularize and use in practical production.
Description
Technical field
The present invention relates to rice quality assessment technique field, identify rice processing accuracy particularly to a kind of gas chromatography
Method.
Background technology
Rice is one of China's Three major grain crops, and the whole nation about 2/3rds population is with rice as staple food.Oryza glutinosa is through rice huller
Paddy, milling work order obtain rice.Rice processing accuracy mainly differentiates according to the residual degree of rice germ surface bran layer, with processing
Precision improves constantly, and its organoleptic quality improves therewith；But it is present in lipid in bran coat, protein, mineral and Wei Sheng
Cellulose content constantly reduces, and causes nutrient loss.Therefore we need to set up one kind can objective, accurately reflect rice processing
The method of precision, retains its nutritional labeling on the premise of ensureing its organoleptic quality as far as possible.
At present, main to the evaluation of rice processing accuracy or based on subjective assessment, that is, pass through to observe from different perspectives
Rice sample, and compare with standard specimen, empirically draw the machining accuracy of rice sample.The method is mainly with GB GB/T
Second method in 5502-2008, that is, " staining " is foundation, and subjectivity is strong, and reviewer needs to train through Professional knowledge
Instruction.Also have in prior art and some parameters of rice and rice processing accuracy are set up correlation model, by detecting the phase of rice
Answer parameter, obtain rice processing accuracy, such as analyze rice external fat content and color using near-infrared spectrum technique, can be very
Predict well rice processing accuracy.But the work difficulty setting up model in the method is big, it is desirable to have the professional of experience and big
The representational sample of amount, and it is equipped with accurate chemical analyses means；And each model can only adapt to the regular hour and
It is therefore desirable to constantly safeguard to model, the technology of user can affect the using effect of model, practical application mistake to spatial dimension
In journey, limitation is larger.
Content of the invention
It is an object of the invention to provide a kind of method that rice processing accuracy identified by gas chromatography, by measuring rice
Middle fat content can precise Identification rice processing accuracy, and simple to operate, time-consuming short, being easy to promote in actual production makes
With.
The invention provides a kind of method that rice processing accuracy identified by gas chromatography, comprise the following steps：
(1) using organic solvent, rice sample is extracted, be extracted liquid, described extract includes fat, institute
Stating fat is fatty acid, a sweet ester, DAG and sweet three esters；
(2) extract obtaining described step (1) carries out gas chromatographic analysiss, obtains the percent mass of fat in rice
Content；The weight/mass percentage composition of described fat is fatty acid, the gross mass percentage composition of a sweet ester, DAG and sweet three esters；
(3) weight/mass percentage composition of fat and predetermined normal equation in the rice being obtained according to described step (2), obtain
The machining accuracy of described rice sample, described normal equation be with rice fat weight/mass percentage composition as independent variable, rice
Grade is the equation of dependent variable, evaluates rice processing accuracy with described rice grade.
Preferably, described normal equation is shown in formula I：
N=0.18+3.44 (TLC) -0.68 (TLC)2Formulas I
In Formulas I, N rice grade, value is 1,2,3 or 4；
TLC based on accounting for rice butt quality, in rice fat weight/mass percentage composition.
Preferably, the described organic solvent of step (1) is polar organic solvent and/or non-polar organic solvent.
Preferably, the granularity of the described rice sample of step (1)<0.45mm.
Preferably, the described extraction of step (1) is carried out under the conditions of vortex oscillation, and extraction time is 0.1～30min.
Preferably, the injector temperature of the described gas chromatographic analysiss of step (2) is 378～382 DEG C, and split ratio is 5:1.
Preferably, the detector of the described gas chromatographic analysiss of step (2) be fid detector, detector temperature be 378～
382℃.
Preferably, the heating schedule of the described gas chromatographic analysiss of step (2) is：
49～51 DEG C of holding 0min, 14～16 DEG C/min are warming up to 178～182 DEG C of holding 1min, and 6～8 DEG C/min heats up
To 228～232 DEG C of holding 0min, 29～31 DEG C/min is warming up to 355～365 DEG C of holding 10min.
Preferably, the flow rate of carrier gas of the described gas chromatographic analysiss of step (2) is 4.3～4.5mL/min, and air velocity is
290～310mL/min, hydrogen flow rate is 29～31mL/min.
Preferably, the chromatographic column of the described gas chromatographic analysiss of step (2) is DB-1HT chromatographic column.
The invention provides the method that rice processing accuracy identified by gas chromatography, using organic solvent, rice sample is entered
Row extraction, is extracted liquid, and described extract includes fat, and described fat is fatty acid, a sweet ester, DAG and sweet three
Ester；The extract obtaining is carried out gas chromatographic analysiss, obtains the weight/mass percentage composition of fat described in rice；According to obtain
In rice, the weight/mass percentage composition of fat and predetermined normal equation, obtain the machining accuracy of described rice sample, described standard
Equation is the equation that weight/mass percentage composition is as independent variable, rice grade is as dependent variable of the fat with rice, with described rice etc.
Level evaluates rice processing accuracy.The present invention establishes the mass content of fat and the quantitative relationship of rice grade in rice, passes through
Measure fat content identification rice processing accuracy in rice, method is accurate and simple to operate, and being easy to promote in actual production makes
With.
Brief description
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the gas chromatogram of Semen oryzae sativae sample；
Fig. 2 is the gas chromatogram of Oryza glutinosa sample；
Fig. 3 is the gas chromatogram of Semen Oryzae sample；
Fig. 4 is the gas chromatogram of fatty acid standard liquid；
Fig. 5 is the gas chromatogram of a sweet ester standard liquid；
Fig. 6 is the gas chromatogram of DAG standard liquid；
Fig. 7 is the gas chromatogram of sweet three ester standard liquids；
Fig. 8 is the gas chromatogram of normal hexane.
Specific embodiment
The invention provides a kind of method that rice processing accuracy identified by gas chromatography, comprise the following steps：
(1) using organic solvent, rice sample is extracted, be extracted liquid, described extract includes fat, institute
Stating fat is fatty acid, a sweet ester, DAG and sweet three esters；
(2) extract obtaining described step (1) carries out gas chromatographic analysiss, obtains the percent mass of fat in rice
Content；The weight/mass percentage composition of described fat is fatty acid, the gross mass percentage composition of a sweet ester, DAG and sweet three esters；
(3) weight/mass percentage composition of fat and predetermined normal equation in the rice being obtained according to described step (2), obtain
The machining accuracy of described rice sample, described normal equation be with rice fat weight/mass percentage composition as independent variable, rice
Grade is the equation of dependent variable, evaluates rice processing accuracy with described rice grade.
The present invention is extracted to rice sample using organic solvent, is extracted liquid, and described extract includes fat,
Described fat is fatty acid, a sweet ester, DAG and sweet three esters.The present invention for described organic solvent species do not have special
Limit, the fatty ingredient in rice sample can be extracted using organic solvent well known to those skilled in the art, specifically
As ether, isobutyltrimethylmethane., pentane, normal hexane, hexamethylene, acetone, ethyl acetate, propyl acetate, isopropanol, isobutanol, benzene, first
In benzene, dimethylbenzene, petroleum ether any one, two or three of combination.Present invention preferably employs those skilled in the art are ripe
The chromatographically pure organic solvent known.
In the present invention, the granularity of described rice sample is preferred<0.45mm, more preferably<0.30mm, most preferably<0.15mm.
Rice to be measured is preferably pulverized by the present invention, crosses 40～140 mesh sub-sieves, the lower part of screen obtaining is allocated as rice sample.This
The bright species for described rice to be measured does not have special restriction, using rice species well known to those skilled in the art is
Can, such as Semen oryzae sativae, Semen Oryzae or Oryza glutinosa.In the present invention, described Semen oryzae sativae preferably specifically includes milled early medium to short-grain nonglutinous rice or late Semen oryzae sativae；Described Semen Oryzae is excellent
Choosing specifically includes early rice or late Semen Oryzae；Described Oryza glutinosa preferably specifically includes milled round grain glutinous rice or Xian Oryza glutinosa.
In the present invention, the volume ratio carrying out quality and the organic solvent of rice sample during described extraction be preferably (0.1～
5.0)g：(0.1～20.0) mL, more preferably (0.5～3.5) g：(1.0～15.0) mL, most preferably (1.5～2.5) g：
(4.5～12.5) mL.In the present invention, described extraction is carried out preferably under the conditions of vortex oscillation；Extraction time be preferably 0.1～
30min, more preferably 1～25min, most preferably 2～15min.
After being extracted liquid, described extract is carried out gas chromatographic analysiss by the present invention, obtains the quality of fat in rice
Percentage composition；The weight/mass percentage composition of described fat is fatty acid, the gross mass percentage of a sweet ester, DAG and sweet three esters contains
Amount.Before carrying out described gas chromatographic analysiss, the present invention preferably removes and derives from rice sample itself and institute in described extract
With contained moisture in organic solvent.The present invention does not have special restriction for the method removing described moisture, using this area
The technical scheme removing moisture removal known to technical staff.Water absorbing agent is preferably mixed by the present invention with described extract, absorbs
Moisture in described extract.The present invention does not have special restriction to the species of described water absorbing agent, ripe using those skilled in the art
That knows has absorptive material, such as anhydrous sodium sulfate.
After removing moisture in described extract, the present invention takes supernatant to cross 0.45 after preferably staticly settling the feed liquid obtaining
μm filter membrane, as gas chromatographic analysiss testing sample.
Present invention preferably employs Agilent 7890B gas chromatograph carries out described gas chromatographic analysiss.In the present invention, institute
The injector temperature stating gas chromatographic analysiss is preferably 378～382 DEG C, more preferably 380 DEG C；Split ratio is preferably 5:1.
In the present invention, the heating schedule of described gas chromatographic analysiss is preferably：49～51 DEG C of holding 0min, 14～16
DEG C/min be warming up to 178～182 DEG C holding 1min, 6～8 DEG C/min be warming up to 228～232 DEG C holding 0min, 29～31 DEG C/
Min is warming up to 355～365 DEG C of holding 10min；More preferably 50 DEG C holding 0min, 15 DEG C/min are warming up to 180 DEG C of holdings
1min, 7 DEG C/min are warming up to 230 DEG C of holding 0min, and 30 DEG C/min is warming up to 360 DEG C of holding 10min.
In the present invention, the carrier gas of described gas chromatographic analysiss is preferably nitrogen, and purity is preferably greater than 99.999%.At this
In invention, the flow rate of carrier gas of described gas chromatographic analysiss is preferably 4.3～4.5mL/min, more preferably 4.41mL/min；Air
Flow velocity is preferably 290～310mL/min, more preferably 300mL/min；Hydrogen flow rate is preferably 29～31mL/min, more preferably
For 30mL/min.
In the present invention, the detector of described gas chromatographic analysiss is preferably fid detector；Detector temperature is preferably
378～382 DEG C, more preferably 380 DEG C.
In the present invention, the chromatographic column of described gas chromatographic analysiss is preferably DB-1HT chromatographic column.
After obtaining gas chromatographic analysiss result, the standard preferably according to the chromatogram obtaining and described fat content for the present invention
Curve, obtains the weight/mass percentage composition of fat in rice sample.In the present invention, the standard curve of described fat content is fat
The standard curve of mass content and chromatographic peak area, the sweet ester specifically being obtained by described gas chromatographic analysiss, DAG,
Sweet three esters and the gas chromatogram peak area of fatty acid, obtain a sweet ester, DAG, sweet three esters and the respective quality of fatty acid hundred
Divide content, and then obtain a sweet ester, the gross mass percentage composition of DAG, sweet three esters and fatty acid, be i.e. the percent mass of fat
Content.
In the present invention, the method setting up sweet three ester standard curves preferably includes following steps：
The sweet three ester standard liquids of variable concentrations gradient are provided；
The sweet three ester standard liquids of described variable concentrations gradient are carried out gas chromatographic analysiss respectively, with peak area as vertical coordinate,
Concentration is abscissa, and peak area is made linear equation to concentration, obtained sweet three ester standard curves.
Present invention firstly provides the sweet three ester standard liquids of variable concentrations gradient.The present invention is for solvent in described sweet three ester standard liquids
Species there is no special restriction, using the solvent for preparing sweet three ester standard liquids well known to those skilled in the art.?
In embodiments of the invention, specifically adopting sweet three esters, fatty acid mark song to adopt chromatographically pure normal hexane is solvent, DAG, Gan Yi
It is solvent that ester mark song adopts chromatographically pure chloroform.The present invention preferably first prepares sweet three ester storing solutions, then described in gradient dilution
Sweet three ester storing solutions, obtain the sweet three ester standard liquids of variable concentrations gradient.The present invention does not have for the method preparing sweet three ester storing solutions
There is special restriction, using the technical scheme preparing solution well known to those skilled in the art.In embodiments of the invention
In, the mass concentration of described sweet three ester storing solutions is specially 25mg/mL.The present invention is for sweet three obtaining after described gradient dilution
The concentration of ester standard liquid does not have special restriction, using the technical scheme of gradient dilution well known to those skilled in the art.?
In embodiments of the invention, obtaining mass concentration particular by gradient dilution is 10mg/mL, 5mg/mL, 3mg/mL, 1mg/
The sweet three ester standard liquids of mL, 0.6mg/mL, 0.4mg/mL, 0.2mg/mL, 0.1mg/mL.
After obtaining the sweet three ester standard liquids of variable concentrations gradient, the sweet three ester standard liquids of described variable concentrations gradient are divided by the present invention
Do not carry out gas chromatographic analysiss, with peak area as vertical coordinate, concentration is abscissa, and peak area is made linear equation to concentration, obtained
Sweet three ester standard curves.In the present invention, the condition of described gas chromatographic analysiss is preferably surveyed with the application technique scheme
The gas chromatographic analysiss determining to adopt during rice sample consistent.In an embodiment of the present invention, described gas chromatographic analysiss
Condition specific as follows：
Using Agilent DB-1HT chromatographic column；380 DEG C of injector temperature；Column temperature program heats up：50 DEG C of holding 0min, 15
DEG C/min is warming up to 180 DEG C of holding 1min, 7 DEG C/min is warming up to 230 DEG C, and 30 DEG C/min is warming up to 360 DEG C of holding 10min；Inspection
Survey device is fid detector, 380 DEG C of temperature；Carrier gas is nitrogen (purity is more than 99.999%), and flow rate of carrier gas 4.41ml/min is empty
Gas velocity 300ml/min, hydrogen flow rate 30.00ml/min；Split ratio 5:1；Sample size 1 μ L.
The present invention, preferably according to the method setting up sweet three ester standard curves, sets up DAG, a sweet ester and Fatty acid standards
Curve.
In an embodiment of the present invention, described sweet three esters, DAG, a sweet ester and fatty acid calibration curve equation concrete
See table：
Wherein, x is respectively sweet three esters, the mass concentration of DAG, a sweet ester and fatty acid, and y corresponds to sweet three esters, sweet respectively
The gas chromatogram peak area of diester, a sweet ester and fatty acid.
According to the calibration curve equation of described fatty acid, a sweet ester, DAG and sweet three esters, fat in liquid can be extracted
The mass concentration of sour, the sweet ester of fat, DAG and sweet three esters, is calculated as C respectivelyx1、Cx2、Cx3And Cx4；According to extract volume with greatly
Rice sample butt quality, formula as shown in Formula II, the weight/mass percentage composition that can obtain in rice fat is (by accounting for rice butt matter
Gauge)：
TLC=(Cx1+Cx2+Cx3+Cx4) × v ÷ m × 100% Formula II
In Formula II, TLC based on accounting for rice butt quality, in rice fat weight/mass percentage composition；
Cx1、Cx2、Cx3And Cx4Fatty acid, the mass concentration of a sweet ester, DAG and sweet three esters in extract；
The volume of v extract；
M rice sample butt quality.
In the present invention, described rice sample butt quality specifically refers to the quality after rice sample removes moisture, described
The moisture of rice sample is measured with reference to the solid sample drying meanss in direct drying method in GB 5009.3-2016.
After obtaining the weight/mass percentage composition of fat in rice, the present invention is according to the weight/mass percentage composition of fat in described rice
With predetermined normal equation, obtain the machining accuracy of described rice sample, described normal equation is with the quality of fat in rice
Percentage composition is independent variable, rice grade is the equation of dependent variable, evaluates rice processing accuracy with described rice grade.The present invention
Preferably the rice that processing grade is one-level, two grades, three-level and level Four is pulverized respectively and crossed 40～140 mesh sub-sieves, obtain
Lower part of screen is allocated as Standard for Rice sample, then according to technique scheme of the present invention is extracted and gas chromatographic analysiss, obtaining
The weight/mass percentage composition (based on accounting for Standard for Rice sample butt quality) of fat in the Standard for Rice sample of different processing grades,
With in Standard for Rice sample, as independent variable, the processing grade of Standard for Rice sample is dependent variable to the weight/mass percentage composition of fat, enters
Row nonlinear fitting, obtains normal equation shown in formula I：
N=0.18+3.44 (TLC) -0.68 (TLC)2Formulas I
In Formulas I, N rice grade, value is 1,2,3 or 4；
TLC based on accounting for rice butt quality, in rice fat weight/mass percentage composition.
Below in conjunction with the embodiment in the present invention, the technical scheme in the present invention is clearly and completely described.Aobvious
So, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the reality in the present invention
Apply example, the every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, all belong to
In the scope of protection of the invention.
Embodiment 1
(1) foundation of standard curve
The foundation of sweet three ester standard curves：Weigh the sweet three ester standard specimens of 0.625g (being accurate to 0.0001g) to hold in 25mL brown
In measuring bottle, add chromatographically pure normal hexane to graduation mark, shake up, obtain the sweet three ester storing solutions of 25mg/mL, gradient dilution obtains concentration
Sweet three ester marks for 10mg/mL, 5mg/mL, 3mg/mL, 1mg/mL, 0.6mg/mL, 0.4mg/mL, 0.2mg/mL, 0.1mg/mL
Liquid；Described sweet three ester standard liquids are carried out gas chromatographic analysiss, with peak area as vertical coordinate, concentration is abscissa, and peak area is to dense
Degree makees linear equation, obtains sweet three ester standard curves；Wherein, the condition of described gas chromatographic analysiss is as follows：
Using Agilent DB-1HT chromatographic column；380 DEG C of injector temperature；Column temperature program heats up：50 DEG C of holding 0min, 15
DEG C/min is warming up to 180 DEG C of holding 1min, 7 DEG C/min is warming up to 230 DEG C, and 30 DEG C/min is warming up to 360 DEG C of holding 10min；Inspection
Survey device is fid detector, 380 DEG C of temperature；Carrier gas is nitrogen (purity is more than 99.999%), and flow rate of carrier gas 4.41ml/min is empty
Gas velocity 300ml/min, hydrogen flow rate 30.00ml/min；Split ratio 5:1；Sample size 1 μ L.
Method according to setting up sweet three ester standard curves, sets up DAG, a sweet ester and Fatty acid standards curve.
Sweet three esters of table 1, the calibration curve equation of DAG, a sweet ester and fatty acid
(2) rice sample preparation
Process of milling after Oryza sativa L. raw material sources and shelling is as follows：
Long-grained nonglutinous rice (Guangdong, 2014 harvest, process time of milling be respectively 30s, 60s, 90s, 120s, 150s, 180s,
210s、240s、270s、300s、340s)；
Japonica rice (Henan, 2014 harvest, process time of milling be respectively 10s, 20s, 30s, 40s, 50s, 60s, 70s,
80s、90s、100s、110s、120s、130s、140s、150s、160s)；
Round-grained rice Oryza sativa L. var. glutinosa Matsum. (Anhui, 2014 harvest, process time of milling be respectively 10s, 30s, 50s, 70s, 90s, 110s,
130s、150s、170s、190s).
Mill after process, the rice obtaining is pulverized and crosses 120 mesh sub-sieves, the lower part of screen obtaining is allocated as rice sample
Product.
(3) extract
The 3mL normal hexane pipetting and accurately the 1g accurately weighing rice sample is placed in test tube (1.5cm × 25cm), rotation
Whirlpool oscillation extraction 3min, adds anhydrous sodium sulfate to remove moisture, takes supernatant to cross 0.45 μm of filter membrane, as gas phase after staticly settling
Chromatography testing sample is transferred in gas phase bottle.
(4) gas chromatographic analysiss
According to GC conditions during Criterion curve, gas chromatographic analysiss are carried out to testing sample, before record
The spectrogram of 23min, is calculated each dense in extracting solution by the standard curve of fatty acid, a sweet ester, DAG and sweet three esters
Degree, and then obtain the weight/mass percentage composition (based on accounting for rice butt quality) of fat in rice sample.
(5) checking of gas Chromatographic Determination result
Measure crude fat content in rice sample using soxhlet extraction methods in GB GB/T 5512-2008, verify the present invention
(described in GB GB/T 5512-2008, crude fat mainly includes glyceride, fat to the accuracy of middle gas Chromatographic Determination result
Acid, phospholipid, glycolipid, but in rice, phospholipid and glycolipid component content are very low, therefore can be with Soxhlet in GB GB/T 5512-2008
Extraction process verifies the accuracy of gas Chromatographic Determination result in the present invention).The results are shown in Table 2～4.
(6) foundation of normal equation and checking
Semen Oryzae, Semen oryzae sativae and Oryza glutinosa (processing grade is one-level, two grades, three-level and level Four) are pulverized respectively and crossed 120 mesh and divides
Sample sieves, and the lower part of screen obtaining is allocated as standard sample, then according to the method described in step (3) and step (4), obtains different adding
In the Semen Oryzae of work grade, Semen oryzae sativae and Oryza glutinosa standard sample, the weight/mass percentage composition of fat is (by accounting for Semen Oryzae, Semen oryzae sativae and Oryza glutinosa standard sample
Product butt quality meter), with Semen Oryzae, Semen oryzae sativae and Oryza glutinosa standard sample fat weight/mass percentage composition as independent variable, Semen Oryzae, Semen oryzae sativae
Processing grade with Oryza glutinosa standard sample is dependent variable, carries out nonlinear fitting, obtains normal equation shown in formula I：
N=0.18+3.44 (TLC) -0.68 (TLC)2Formulas I
In Formulas I, N rice grade, value is 1,2,3 or 4；
TLC based on accounting for Semen Oryzae, Semen oryzae sativae and Oryza glutinosa standard sample butt quality, Semen Oryzae, Semen oryzae sativae and Oryza glutinosa standard sample
The weight/mass percentage composition of middle fat.
According to the weight/mass percentage composition of fat in the rice sample that step (4) obtains, using the normal equation pair shown in Formulas I
Rice sample is classified, and is verified (the results are shown in Table 2～4) using staining in GB/T 5502-2008.
Table 2 Semen Oryzae grade, fat content gas chromatographic analysiss measured value and soxhlet type measured value
Table 3 Semen oryzae sativae grade, fat content gas chromatographic analysiss measured value and soxhlet type measured value
Table 4 Oryza glutinosa grade, fat content gas chromatographic analysiss measured value and soxhlet type measured value
From data above, the present invention is by detecting that using gas chromatographic analysiss the percent mass of fat in rice contains
Amount, compared with soxhlet extraction methods in GB GB/T 5512-2008, simple to operate, time-consuming short, organic solvent usage amount is little, but
Testing result accurately, disclosure satisfy that and is actually needed.Meanwhile, the present invention with rice fat weight/mass percentage composition as independent variable,
Rice grade is dependent variable, and Criterion equation evaluates rice processing accuracy with described rice grade, and authentication method accurately, is kept away
Exempt from staining subjectivity in GB/T 5502-2008 strong, difficulty set up by other models related to rice processing accuracy, and comments
Survey personnel need the problem through Professional knowledge training, are easy to promote the use of in actual production.
The above is only the preferred embodiment of the present invention it is noted that ordinary skill people for the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. the method that rice processing accuracy identified by gas chromatography, comprises the following steps：
(1) using organic solvent, rice sample is extracted, be extracted liquid, described extract includes fat, described fat
Fat is fatty acid, a sweet ester, DAG and sweet three esters；
(2) extract obtaining described step (1) carries out gas chromatographic analysiss, and the percent mass obtaining fat in rice contains
Amount；The weight/mass percentage composition of described fat is fatty acid, the gross mass percentage composition of a sweet ester, DAG and sweet three esters；
(3) weight/mass percentage composition of fat and predetermined normal equation in the rice being obtained according to described step (2), obtain described
The machining accuracy of rice sample, described normal equation be with rice fat weight/mass percentage composition as independent variable, rice grade
For the equation of dependent variable, rice processing accuracy is evaluated with described rice grade.
2. method according to claim 1 it is characterised in that described normal equation shown in formula I：
N=0.18+3.44 (TLC) -0.68 (TLC)2Formulas I
In Formulas I, N rice grade, value is 1,2,3 or 4；
TLC based on accounting for rice butt quality, in rice fat weight/mass percentage composition.
3. method according to claim 1 it is characterised in that the described organic solvent of step (1) be polar organic solvent and/
Or non-polar organic solvent.
4. method according to claim 1 is it is characterised in that the granularity of the described rice sample of step (1)<0.45mm.
5. method according to claim 1 it is characterised in that step (1) described extraction carry out under the conditions of vortex oscillation,
Extraction time is 0.1～30min.
6. method according to claim 1 is it is characterised in that the injector temperature of the described gas chromatographic analysiss of step (2)
For 378～382 DEG C, split ratio is 5:1.
7. method according to claim 6 is it is characterised in that the detector of the described gas chromatographic analysiss of step (2) is FID
Detector, detector temperature is 378～382 DEG C.
8. method according to claim 7 is it is characterised in that the heating schedule of the described gas chromatographic analysiss of step (2) is：
49～51 DEG C of holding 0min, 14～16 DEG C/min are warming up to 178～182 DEG C of holding 1min, and 6～8 DEG C/min is warming up to 228
～232 DEG C of holding 0min, 29～31 DEG C/min are warming up to 355～365 DEG C of holding 10min.
9. method according to claim 8 is it is characterised in that the flow rate of carrier gas of the described gas chromatographic analysiss of step (2) is
4.3～4.5mL/min, air velocity is 290～310mL/min, and hydrogen flow rate is 29～31mL/min.
10. method according to claim 8 is it is characterised in that the chromatographic column of the described gas chromatographic analysiss of step (2) is
DB-1HT chromatographic column.
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| CN108802303A (en) * | 2018-05-24 | 2018-11-13 | 益阳市福华米业有限公司 | A kind of rice processing accuracy automated detection method |
| CN110412152A (en) * | 2019-06-25 | 2019-11-05 | 北京三聚环保新材料股份有限公司 | A kind of waste animal and vegetable oil hydrogenation products composition analysis method |
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