CN109030658A - The detection method of oligofructose and gossypose in a kind of Milk Powder Formula For Infants - Google Patents
The detection method of oligofructose and gossypose in a kind of Milk Powder Formula For Infants Download PDFInfo
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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
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Abstract
The invention discloses the detection methods of oligofructose and gossypose in a kind of Milk Powder Formula For Infants, comprising the following steps: (1) pre-treatment；(2) configuration of standard solution；(3) liquid chromatogram, regression equation are obtained；(4) qualitative analysis；(5) quantitative to calculate, using quantified by external standard method: the concentration of ketose, Nystose, sugarcane sugar or/and gossypose is calculated using the regression equation of step (3) according to the area of chromatographic peak in sample chromatogram；This research preferably novel hydrophilic separation material, in conjunction with high-efficient liquid phase chromatogram technology, developed it is a kind of it is easy, quickly, the qualitative-and-quantitative method that oligofructose and gossypose detect simultaneously in accurate detection milk power for infant and young children.
Description
Technical field
The present invention relates to the detection methods of oligofructose and gossypose in a kind of Milk Powder Formula For Infants, belong to food inspection technology
Field.
Background technique
Oligofructose (fructo oligosaccharide, FOS) is to pass through β-(2,1) sugar by sucrose and 1 ~ 3 fructose
The ingredients such as the oligosaccharide that glycosidic bond is combined into, including ketose (GF2), Nystose (GF3), sugarcane sugar (GF4).It is oligomeric
Fructose has the growth for promoting intestinal bifidobacteria, adjusts the function of intestinal flora balance.Gossypose (Raffinose) is by half
A kind of functional oligose that lactose, fructose and glucose are combined into, it may have relatively proliferation Bifidobacterium effect by force.Due to baby
The intestinal growth function of youngster is not yet mature, is easy to appear intestinal bacilli illness, and by extraneous viral or bacterium infection, cause
The diseases such as diarrhea.Draw its function of adjusting intestinal flora using oligofructose and gossypose, it is extensive to become dispensed food for baby
One of raw material used plays irreplaceable role in milk power for infant and young children.Oligosaccharide is in dispensed food for baby
In application cause the extensive concern of entire industry.
That reports at present has high performance liquid chromatography, the chromatography of ions, liquid chromatography-mass spectrography to oligofructose detection method
The methods of method, wherein mainly in the majority with the chromatography of ions.The detection of oligofructose is divided into direct Detection Method and indirect detection method.Its
Middle food safety national safety standard GB 5009.255-2016 " measurement of levulan in food " is indirect detection method, is to pass through
Ion-chromatographic determination fructose content is utilized after hydrolysis, obtains oligofructose total amount in food by conversion, is not directed to specific low
The Separation Research of each ingredient of glycan.Direct Detection Method is to calculate adduction after directly measuring each ingredient of oligofructose to obtain total amount.Cause
The main component of added oligofructose is ketose, Nystose, sugarcane sugar, measures these three single components and represents
The addition content of oligofructose.It is food additives, raw material and feed that the direct Detection Method reported at present, which predominantly detects object,
Etc. simple matrix, testing conditions are relatively simple.The method of oligofructose is also reported in the complex matrices such as Milk Powder Formula For Infants, main
To show difference/evaporative light scattering detector method for hydrophilic chromatographic/high performance liquid chromatography-, but all exist and separate bad, serious interference
The problem of.Main cause is that there are the interference of the monosaccharide such as the lactose of high-content in Milk Powder Formula For Infants, the oligomeric fruit with low content
Sugared polarity is suitable, causes separation difficult, the problems such as being quantitatively not allowed.Improve separation problem, main method is optimization pre-treating method
With improvement chromatographic separation condition, oligofructose is that polar compound mainly uses hydrophilic chromatographic column to be separated, and chromatographic condition can
It is smaller to adjust space, the selection of hydrophilic chromatographic column is the key that separation.
The detection method of the gossypose of report has high performance liquid chromatography and the chromatography of ions.Food safety national security mark
Quasi- GB 5009.258-2016 " measurement of gossypose in food " is by protein precipitation, through the chromatography of ions after solid-phase extraction column
Detect gossypose in food.The problems such as that there are qualitative tools is single for this method, and baseline drift is serious, high to instrument requirements.
Gossypose examination criteria is using ion chromatography-ampere detector detection dispensed food for baby, infant's cereal
Accesary foods, the canned accesary foods of infant, beverage and bean powder food.And oligofructose content is surveyed using indirect method in food
It is fixed, and this method operating process is complicated, can only obtain oligosaccharide total amount, can not obtain its specific composition information.
For the method for oligofructose in milk power for infant and young children and gossypose detection simultaneously, there is not been reported at present.In view of
Oligofructose and gossypose adjust the function of intestinal flora, are widely used in milk power for infant and young children, and detection becomes baby
The conventional detection project that child's milk powder quality is checked on and supervised, but need to detect respectively both as different detection methods.
Summary of the invention
The preferably novel hydrophilic separation material of this research has developed a kind of easy, fast in conjunction with high-efficient liquid phase chromatogram technology
The qualitative-and-quantitative method that oligofructose and gossypose detect simultaneously in speed, accurate detection milk power for infant and young children.
To solve the above-mentioned problems, the present invention provides the detection side of oligofructose and gossypose in a kind of Milk Powder Formula For Infants
Method.
The present invention is achieved by the following technical solutions:
The detection method of oligofructose and gossypose in a kind of Milk Powder Formula For Infants, comprising the following steps:
(1) pre-treatment: weighing 1 g sample, is placed in 15 mL centrifuge tubes, adds 5 mL warm water, 80 DEG C of water-bath vibrations after the dissolution that is vortexed
It swings and extracts 30 min, take 1 mL extracting solution in another centrifuge tube, add 3 mL acetonitriles+water, acetonitrile and water volume ratio 2:1, add 0.2
G C18 adsorbent is vortexed, and centrifugation, supernatant crosses 0.22 μm of organic filter membrane, to upper machine；
(2) configuration of standard solution: ketose, Nystose, sugarcane sugar and each reference substance of gossypose are accurately weighed respectively
100 mg of matter dissolves with water and is settled to scale in 10 mL volumetric flasks, 10 mg/mL standard reserving solutions is configured to, in 4 DEG C
Under the conditions of save；Standard reserving solution is prepared into gradient standard working solution with 1:1 acetonitrile-water, is saved under the conditions of 4 DEG C；
(3) liquid chromatogram, regression equation are obtained
Gradient standard working solution is detected with HPLC ELSD detector, chromatogram is obtained, with chromatography
The log value of peak area is ordinate, with ketose in standard working solution, Nystose, sugarcane sugar, gossypose it is corresponding
The log value of concentration value is abscissa mapping, obtains log-log equation of linear regression；
(4) qualitative analysis
Sample is detected with HPLC ELSD detector, obtains sample chromatogram；If in sample chromatogram
In the presence of chromatographic peak corresponding with the chromatographic peak in standard chromatogram；Then show to contain ketose, Nystose, sugarcane fruit in sample
Pentasaccharides, gossypose；
(5) quantitative to calculate
Using quantified by external standard method: being calculated according to the area of chromatographic peak in sample chromatogram using the regression equation of step (3)
To the concentration of ketose, Nystose, sugarcane sugar or/and gossypose；
Ketose, Nystose, sugarcane sugar, the content of gossypose are calculated as follows in sample:
In formula (1):
The content of each determinand in Xi-sample, unit are each hectogram of milligram (mg/100g)；
The concentration of each determinand in c-measurement sample solution, unit are every milliliter of milligram (mg/mL)；
V-constant volume volume, unit are milliliter (mL)；
F-extension rate；
M-sample quality, unit are gram (g)；
Xi is respectively XKetose、XNystose、XSugarcane sugarAnd XGossypose；
The content of oligofructose in sample: XOligofructoseRespectively XKetose+XNystose+XSugarcane sugar。
Preferably, the chromatographic column of the high performance liquid chromatograph: Click XIon, column length 150mm, 3.0 mm of column internal diameter,
3 μm of packing material size (development of the Dalian Chemistry and Physics Institute)；The mobile phase of the ultra performance liquid chromatography: A: acetonitrile, B: water.
It is highly preferred that the elution requirement of the high performance liquid chromatography are as follows: column temperature: 40 DEG C, sampling volume: 5 μ L；Gradient is washed
De- condition is as follows:
" gradient 6 " refers to that gradient is straight line.
Preferably, the parameter of the Evaporative light scattering detector instrument: 80 DEG C of drift tube temperature, 30 psi of nitrogen pressure, spray
60 DEG C of day with fog temperature, gain 50.
The present invention establishes while measuring the analysis method of oligofructose and gossypose in Milk Powder Formula For Infants.Sample is using temperature
Water extracts, acetonitrile precipitation albumen, using hydrophilic chromatographic column Click Xion(100mm × 2.1mm i.d., 5 μm of partial size) separation,
Gradient elution is carried out by mobile phase of acetonitrile-water, evaporative light scattering detector is measured.It is molten to investigate and optimize herein extraction
Agent, purification style, ELSD condition and chromatographic condition etc., ELSD optimal conditions figure are shown in Fig. 4.The result shows that: oligofructose and cotton seed
Sugar (ketose, Nystose 0.02-2 mg/mL, sugarcane sugar and gossypose 0.01-2 mg/mL) in respective range has
There is preferable linear relationship, related coefficient is greater than 0.998.Under high, normal, basic three pitch-based spheres, the rate of recovery of actual sample exists
Between 87.4 %~104.5%, relative standard deviation (n=6 RSD) between 2.9 %-8.5%, ketose and Nystose
Detection is limited to 18 mg/100g, and lower limit of quantitation is 40 mg/100g, and the detection of sugarcane sugar and gossypose is limited to 10 mg/100g,
Lower limit of quantitation is 30 mg/100g.Pre-treatment of the present invention is simple and quick, and hydrophilic chromatographic post separation effect is good, can be preferably oligomeric
Fructose (ketose, Nystose, sugarcane sugar) and gossypose are separated with interference monosaccharide components, and high sensitivity is qualitative fixed
Amount is accurate.The present invention can in fabulous realizations Milk Powder Formula For Infants the accurate quantitative analysis of oligofructose and gossypose with detect simultaneously, mention
High detection efficiency reduces testing cost.
Beneficial effect
(1) it realizes and efficiently separates and accurate quantitative analysis
For oligosaccharide as a kind of water soluble ingredient, polarity is stronger, does not retain on general reverse-phase chromatography.Various hydrophilic interactions
Chromatography can provide suitable reservation for highly polar and strongly hydrophilic compound.The monosaccharide and disaccharides such as lactose in Milk Powder Formula For Infants
Content is higher, seriously affects the analysis detection of low content oligosaccharide.The detection of oligofructose in Milk Powder Formula For Infants reported in the literature
, quantitatively there are serious problems in all not up to preferable separation.The present invention is respectively compared Xbrige Amide, NH2 column and Click
It is strong to show that Click XIon chromatographic column retains by comparing for several hydrophilic chromatographic columns such as XIon, can within a short period of time well
Low content oligofructose is effectively separated with high levels of sugars such as lactose, is particularly suitable for point of oligosaccharide in milk power for infant and young children
Analysis, compares chromatogram and sees Fig. 2.It can be seen that the present invention realize oligofructose with interference component be kept completely separate and it is accurately fixed
Amount realizes precisely detection and quality control.
(2) detection efficiency is improved
Round of visits needed for GB 5009.255-2016 " measurement of levulan in food " detects oligofructose is about 300 min,
Wherein sample extraction and purification need 250 min, and detection at least needs 50min；GB 5009.258-2016 " gossypose in food
Measurement " survey gossypose needed for round of visits be about 100 min, wherein sample extraction and purification need 90 min, detection at least
Need 50 min.The pre-treatment time of the present invention only needs 50 min, 30 min of Instrument measuring, and entire round of visits needs 80 min.
It can be seen that the present invention can greatly improve checkability.If carrying out mass detection, the high advantage of checkability will be brighter
It is aobvious.
(3) detection efficiency is improved
The detection of ketose and Nystose is limited to 18 mg/100g in the present invention, and lower limit of quantitation is 40 mg/100g, sugarcane fruit
The detection of pentasaccharides and gossypose is limited to 10 mg/100g, and lower limit of quantitation is 30 mg/100g.National standard is fully met to oligomeric
The requirement of fructose (ketose, Nystose, sugarcane sugar) and gossypose, and detection limit reports water not higher than existing literature
Flat, even lower than document detection limit in part is horizontal.
(4) testing cost is reduced
The present invention merges into the inspection twice of oligofructose (ketose, Nystose, sugarcane sugar) and gossypose once
Experiment, and without digesting and crossing Solid phase extraction, greatly reduce experimental cost.The present invention and GB 5009.255-2016 and
GB 5009.258-2016 is compared, and instrument testing cost is suitable, only calculates pre-treatment cost.GB 5009.255-2016 detection is low
The each testing expenses of Fructooligosaccharides are greater than 50 yuan；It is about 50 yuan that GB 5009.258-2016, which detects each testing expenses of gossypose,；Cause
This, detects oligofructose by several times and gossypose pre-treatment expense is 100 yuan altogether.And pre-treatment expense of the present invention only needs 10 yuan.Than
Compared with discovery, pre-treatment cost of the present invention reduces by ten times or more, also reduces once upper machine testing cost.
Detailed description of the invention
Fig. 1 is Milk Powder Formula For Infants sample chromatogram figure under Xbrige Amide chromatographic column；
Fig. 2 is Milk Powder Formula For Infants sample chromatogram figure under Click XIon chromatographic column；
Fig. 3 is the chromatogram of 4 kinds of oligosaccharide standard solution；
Fig. 4 is 4 kinds of oligosaccharide ELSD condition optimizing figures (A: drift tube temperature optimization figure；B: sprayer temperature optimization figure；C: nitrogen
Atmospheric pressure optimization figure；D: gain optimization figure).
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
1, instrument and material
Waters H-CLASS Ultra Performance Liquid Chromatography instrument matches ACQUITY UPLC ELS detector (Waters, US)；
Chromatographic column: Click XIon chromatographic column (the mm i. of 150 mm × 3.0 d, 3 μm).
Ketose, Nystose, sugarcane sugar standard substance are Japan's Wako standard substance suit, and purity is
99.9%, gossypose is purchased from Sigma, and purity >=99.5%, 4 DEG C saves；Acetonitrile (chromatographically pure, Fisher company of the U.S.)；Water is super
Pure water；Nitrogen (> 99.999%)；C18 adsorbent (Agilent company of the U.S.).(0.22 μm, be purchased from Shanghai to organic miillpore filter
An Pu scientific instrument Co., Ltd).
2, pre-treatment
2.1 standard reserving solution
Oligofructose (ketose, Nystose, sugarcane sugar) and each 100 mg of standard substance of gossypose are accurately weighed respectively
Scale is dissolved with water and be settled to (being accurate to 0.1mg) in 10 mL volumetric flasks, is configured to 10 mg/mL standard reserving solutions, in
It is saved under the conditions of 4 DEG C.
2.2 standard working solution
Standard reserving solution is prepared into gradient standard working solution with 1:1 acetonitrile-water, is saved under the conditions of 4 DEG C.
2.3 sample
Weigh 1 g(and be accurate to 0.1 mg) sample, it is placed in 15 mL centrifuge tubes, adds 5 mL warm water, 80 DEG C of water after the dissolution that is vortexed
30 min of mechanical shaking extraction is bathed, takes 1 mL extracting solution in another centrifuge tube, adds 3 mL acetonitriles+water (volume ratio 2+1), add 0.2 g
C18 adsorbent is vortexed, and centrifugation, supernatant crosses 0.22 μm of organic filter membrane, to upper machine.
3, liquid phase chromatogram condition
3.1 chromatographic condition
Chromatographic column: Click XIon, column length 150mm, column internal diameter 3.0mm, 3 μm of packing material size；
Mobile phase: A: acetonitrile, B: water；
Gradient elution, gradient condition are shown in Table 1, column temperature: 40 DEG C, sampling volume: 5 μ L；
1 liquid chromatogram gradient condition of table
" gradient 6 " refers to that gradient is straight line.
3.2 ELSD conditions
80 DEG C of drift tube temperature, 30 psi of nitrogen pressure, 60 DEG C of sprayer temperature, gain 50.
(2) liquid chromatogram, regression equation are obtained
Gradient standard working solution is detected with HPLC ELSD detector, obtains chromatogram；
Using the log value of chromatographic peak area as ordinate, with oligofructose in standard working solution (ketose, Nystose, sugarcane
Fruit pentasaccharides), the log value of the respective concentration value of gossypose be abscissa mapping, obtain log-log equation of linear regression；
(3) qualitative analysis
Sample is detected with HPLC ELSD detector, obtains sample chromatogram；If in sample chromatogram
In the presence of chromatographic peak corresponding with the chromatographic peak in standard chromatogram；Then show to contain oligofructose (ketose, sugarcane fruit in sample
Tetrose, sugarcane sugar), gossypose；
(4) quantitative to calculate
Using quantified by external standard method: being calculated according to the area of chromatographic peak in sample chromatogram using the regression equation of step (2)
To oligofructose (ketose, Nystose, sugarcane sugar) or/and the concentration of gossypose；
4, standard quality chromatogram and line regression equation
With HPLC ELSD detector, according to the condition of step 3, metric works solution is obtained different
The chromatogram (standard chromatogram) of the standard working solution of concentration.The standard of one of concentration level (0.5 mg/mL) works
The chromatogram of solution is as shown in Figure 3.
Standard working solution is pressed into mass concentration sequentially determining from low to high, with the log value of each oligosaccharide peak area Y to it
Mass concentration X(μ g/mL) log value make standard curve, obtain each oligosaccharide log-log linear equation, the range of linearity and correlation
Coefficient the results are shown in Table 2.As can be seen from Table 2, oligofructose and gossypose (ketose, Nystose 0.02-2 in respective range
Mg/mL, sugarcane sugar and gossypose 0.01-2 mg/mL) there is preferable linear relationship, related coefficient is greater than 0.998.It is to be measured
Oligofructose (ketose, Nystose, sugarcane sugar) and gossypose response should be in the standard curve ranges of linearity in sample
It is interior, it is analyzed again after should then being diluted more than the range of linearity.
24 kinds of oligosaccharide equations of linear regression of table
5, the method rate of recovery, precision and detection limit
2 parts will be divided into a milk power for infant and young children sample, a copy of it makees background, another adds low middle high three concentration
Horizontal standard solution, is detected according to step 4, and every part of sample carries out 6 parallel determinations, investigates the rate of recovery and essence of method
Density the results are shown in Table 2.Statistics indicate that the rate of recovery of this method, between 87.4%~104.5%, relative standard deviation (RSD) is
2.9%~8.5%, the method rate of recovery is high, favorable reproducibility.
The rate of recovery (the rate of recovery: (measured value-of oligofructose (ketose, Nystose, sugarcane sugar) and gossypose
Background values)/additional amount × 100%), the results are shown in Table 3.The rate of recovery is in 87.4%~104.5% range seen from table 3.
To various sample replication 6 times, measurement result all has good reproducibility, oligofructose (ketose, sugarcane
Fruit tetrose, sugarcane sugar) and gossypose relative standard deviation (RSD) be 2.9%~8.5%.
Using the method for adding target compound in blank Milk Powder Formula For Infants, the inspection of ketose and Nystose is measured
Rising limit (S/N > 3) is 18 mg/100g, and lower limit of quantitation (S/N > 10) is 40 mg/100g, the detection of sugarcane sugar and gossypose
It is limited to (S/N > 3) 10 mg/100g, lower limit of quantitation (S/N > 10) is 30 mg/100g.
4 kinds of oligosaccharide TIANZHU XINGNAO Capsuls and precision (n=6) in 3 milk power for infant and young children of table
6, sample detection
(1) qualitative analysis
Sample is detected with HPLC ELSD detector, according to the condition of step 3, is measured sample, is obtained
Sample chromatogram；If there is chromatographic peak corresponding with the chromatographic peak in standard chromatogram in sample chromatogram；Then show in sample
Contain oligofructose (ketose, Nystose, sugarcane sugar), gossypose；
(2) quantitative to calculate
Using quantified by external standard method: being calculated according to the area of chromatographic peak in sample chromatogram using the regression equation of step 4
The concentration of oligofructose (ketose, Nystose, sugarcane sugar) or/and gossypose；
Ketose, Nystose, sugarcane sugar, the content of gossypose are calculated as follows in sample:
In formula (1):
The content of each determinand in Xi-sample, unit are each hectogram of milligram (mg/100g)；
The concentration of each determinand in c-measurement sample solution, unit are every milliliter of milligram (mg/mL)；
V-constant volume volume, unit are milliliter (mL)；
F-extension rate；
M-sample quality, unit are gram (g)；
Xi is respectively XKetose、XNystose、XSugarcane sugarAnd XGossypose；
The content of oligofructose in sample: XOligofructoseRespectively XKetose+XNystose+XSugarcane sugar；
Obviously, those skilled in the art various changes and modifications can be made to the invention without departing from spirit of the invention and
Range.In this way, if these modifications and changes of the present invention is within the scope of the claims of the present invention and its equivalent technology,
Then the present invention is also intended to include these modifications and variations.
Claims (4)
1. the detection method of oligofructose and gossypose in a kind of Milk Powder Formula For Infants, which comprises the following steps:
(1) pre-treatment: weighing 1 g sample, is placed in 15 mL centrifuge tubes, adds 5 mL warm water, 80 DEG C of water-bath vibrations after the dissolution that is vortexed
It swings and extracts 30 min, take 1 mL extracting solution in another centrifuge tube, add 3 mL acetonitriles+water, acetonitrile and water volume ratio 2:1, add 0.2
G C18 adsorbent is vortexed, and centrifugation, supernatant crosses 0.22 μm of organic filter membrane, to upper machine；
(2) configuration of standard solution: ketose, Nystose, sugarcane sugar and each reference substance of gossypose are accurately weighed respectively
100 mg of matter dissolves with water and is settled to scale in 10 mL volumetric flasks, 10 mg/mL standard reserving solutions is configured to, in 4 DEG C
Under the conditions of save；Standard reserving solution is prepared into gradient standard working solution with 1:1 acetonitrile-water, is saved under the conditions of 4 DEG C；
(3) liquid chromatogram, regression equation are obtained
Gradient standard working solution is detected with HPLC ELSD detector, chromatogram is obtained, with chromatography
The log value of peak area is ordinate, with ketose in standard working solution, Nystose, sugarcane sugar, gossypose it is corresponding
The log value of concentration value is abscissa mapping, obtains log-log equation of linear regression；
(4) qualitative analysis
Sample is detected with HPLC ELSD detector, obtains sample chromatogram；If in sample chromatogram
In the presence of chromatographic peak corresponding with the chromatographic peak in standard chromatogram；Then show to contain ketose, Nystose, sugarcane fruit in sample
Pentasaccharides, gossypose；
(5) quantitative to calculate
Using quantified by external standard method: being calculated according to the area of chromatographic peak in sample chromatogram using the regression equation of step (3)
To the concentration of ketose, Nystose, sugarcane sugar or/and gossypose；
Ketose, Nystose, sugarcane sugar, the content of gossypose are calculated as follows in sample:
In formula (1):
The content of each determinand in Xi-sample, unit are each hectogram of milligram (mg/100g)；
The concentration of each determinand in c-measurement sample solution, unit are every milliliter of milligram (mg/mL)；
V-constant volume volume, unit are milliliter (mL)；
F-extension rate；
M-sample quality, unit are gram (g)；
Xi is respectively XKetose、XNystose、XSugarcane sugarAnd XGossypose；
The content of oligofructose in sample: XOligofructoseRespectively XKetose+XNystose+XSugarcane sugar。
2. the method according to claim 1, wherein the chromatographic column of the high performance liquid chromatograph: Click
XIon, 150 mm of column length, 3.0 mm of column internal diameter, 3 μm of packing material size；The mobile phase of the ultra performance liquid chromatography: A: acetonitrile,
B: water.
3. according to the method described in claim 2, it is characterized in that, the elution requirement of the high performance liquid chromatography are as follows: column temperature: 40
DEG C, sampling volume: 5 μ L；Condition of gradient elution is as follows:
" gradient 6 " refers to that gradient is straight line.
4. the method according to claim 1, wherein the parameter of the Evaporative light scattering detector instrument: drift tube
80 DEG C of temperature, 30 psi of nitrogen pressure, 60 DEG C of sprayer temperature, gain 50.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020252677A1 (en) * | 2019-06-19 | 2020-12-24 | 北京三元食品股份有限公司 | High-throughput quantitative determination method of free oligosaccharides in milk |
| CN112649516A (en) * | 2019-10-12 | 2021-04-13 | 中国科学院大连化学物理研究所 | Derivatization-based milk powder containing 4 human milk oligosaccharides and qualitative and quantitative method thereof |
| CN115144494A (en) * | 2022-06-28 | 2022-10-04 | 贵州大学 | Method for detecting oligosaccharide in mammal milk |
| CN116087370A (en) * | 2023-03-06 | 2023-05-09 | 广州汇标检测技术中心 | Method for detecting fructo-oligosaccharide in pet nutrient solution |
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| CN116087370A (en) * | 2023-03-06 | 2023-05-09 | 广州汇标检测技术中心 | Method for detecting fructo-oligosaccharide in pet nutrient solution |
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