CN106198801A - A kind of vitamin D3the detection method of content - Google Patents
A kind of vitamin D3the detection method of content Download PDFInfo
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- CN106198801A CN106198801A CN201610543201.5A CN201610543201A CN106198801A CN 106198801 A CN106198801 A CN 106198801A CN 201610543201 A CN201610543201 A CN 201610543201A CN 106198801 A CN106198801 A CN 106198801A
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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
Abstract
The present invention relates to a kind of vitamin D3The detection method of content, which solves existing vitamin D3The technical problem that the detection method of content scope of application is little, detection efficiency is low and relatively costly, it is by obtaining pretreatment sample liquid after testing sample carries out saponifiable extraction, then use silicagel column Solid phase cleaned-up technology that pretreatment sample liquid is purified or treats sample measuring liquid, finally utilize high-efficient liquid phase chromatogram technology that testing sample is carried out vitamin D3Carry out content qualification, the composite can be widely applied to vitamin D3The detection of content.
Description
Technical field
The present invention relates to the detection method of a kind of content of material, especially relate to a kind of vitamin D3The detection side of content
Method.
Background technology
Vitamin D3For steroid derivant, also known as cholecalciferol, it is mainly derived under dietary int ake or ultraviolet irradiation
Internal synthesis, can promote the absorption of internal calcium constituent, P elements, and the disease causing children rachitis and adult's calcium deficiency can rise
To good preventive effect.Therefore, vitamin D3 be often applied to replenishing the calcium class health food in.China is in health food
Vitamin D3The detection of content does not also provide standard method, along with the detection demand of health food grows with each passing day, the most right
Vitamin D3Detection method mainly have euzymelinked immunosorbent assay (ELISA), high performance liquid chromatography and high performance liquid chromatography tandem mass spectrum method, under
These three method is illustrated by face respectively.
(1) euzymelinked immunosorbent assay (ELISA) is mainly for plasma sample, and its operation and equipment are the most relatively simple, but its scope of application is relatively
Little, it is impossible to the health food complicated to substrate detects.
(2) method of high performance liquid chromatography Main Basis GB5413.9-2010, the method is mainly for infant food
And milk, use the detection of positive-anti-phase dual system, complex steps and operating time length, easily lose, the technology of operator is wanted
Summation Laboratory Instruments condition requires the highest, and operator need to immediately enter positive phase system after obtaining pretreatment sample liquid and divide
From and collect the liquid in the reservation period needed, and give nitrogen at once and blow, total processing time is long, is highly vulnerable to breakage dimension raw
The content of element.Meanwhile, this method is the highest for Laboratory Request, needs to have two liquid phase instruments simultaneously or a set of cuts online
Changing device, expense cost is the highest.
(3) high performance liquid chromatography tandem mass spectrum method mainly uses Isotopic Internal Standard detection, and the method sensitivity is higher, but
Being that isotopic standard is expensive, be not suitable for the detection of a large amount of sample of routine work, the price buying Isotopic Internal Standard exceedes
A lot of times of the testing cost of common laboratory, and domestic there is no manufacturer, need to be from foreign procurement, latent period is the longest.
For this reason, it may be necessary to set up one both economical and convenients and applied widely, the most universal method, is used for detecting sample outstanding
It is vitamin D in health product3Content, for vitamin D3The routine work of detection provides reference method.
Summary of the invention
The present invention is aiming at existing vitamin D3The detection method of content scope of application is little, detection efficiency is low and relatively costly
Technical problem, it is provided that a kind of applied widely, detection efficiency is high and lower-cost vitamin D3The detection method of content.
The present invention provides a kind of vitamin D3The detection method of content, its step is as follows:
(1) preparation of standard solution
Vitamin D is accurately weighed under the conditions of lucifuge3Standard substance, are configured to, with ethanol, the standard that theoretical concentration is 1mg/mL
Storing solution；Draw above-mentioned standard reserving solution appropriate, use methanol dilution to be configured to the standard that concentration is 0.1～5.0 μ g/mL molten
Liquid；
(2) sample treatment
1. saponification: weigh the sample to be detected of mix homogeneously, be sequentially added into ascorbic acid, pyrogallic acid, 2,6-
Ditertbutylparacresol, dehydrated alcohol and potassium hydroxide aqueous solution, carry out saponification under the effect of heating magnetic stirring apparatus；
2. extraction: be transferred in separatory funnel by saponification liquor, adds extractant and extracts, merge the extraction of extraction gained
Agent, is collected in round-bottomed flask after removing trace water；Round-bottomed flask is steamed near dry, then dries up with Nitrogen evaporator；
3. constant volume: by washing the most a small amount of for the round-bottomed flask normal hexane dried up and be transferred in constant volume bottle stand-by；
4. purify: successively with dichloromethane and normal hexane drip washing activated silica gel post, draw the sample liquid after constant volume and transfer to silicon
In glue post, dry up with Nitrogen evaporator after remove impurity, eluting, add methanol and dissolve, by obtaining filtrate after membrane filtration；
(3) high performance liquid chromatograph analysis
Filtrate step 4. obtained is injected high performance liquid chromatograph and is analyzed.
Preferably, in step (3), chromatographic condition is as follows:
Chromatographic column: HPLC SB C18 post (0.45 μm, 5mm × 150mm)；
Flowing phase: the methanol of 95% and the water of 5%；
Flow velocity 0.3mL/min；
Column temperature: 40 DEG C；
UV-detector (DAD) detection wavelength: 264nm；
Sample size is 5 μ L.
Preferably, step (1) uses ethanol stepwise dilution during preparation standard reserving solution, calculate standard storage by extension rate
The actual concentrations of standby liquid, uses spectrophotometer be corrected and calculate correcting fluid reality under 264nm wavelength when calculating concentration
Concentration.
Preferably, step 1. middle ascorbic acid, pyrogallic acid, 2,6 ditertiary butyl p cresol and the mass ratio of sample
It is 1.5: 1: 0.1: 10.
Preferably, in step 1. middle potassium hydroxide aqueous solution, the mass percent of potassium hydroxide is 35%, and saponification temperature is
75 DEG C, saponification time is 40 minutes.
Preferably, step 2. middle extractant is petroleum ether, and extraction times is more than 3 times.
Preferably, normal hexane drip washing is first used during step 4. remove impurity, then with hexamethylene, normal hexane and the mixing of isopropanol
The volume ratio of solution drip washing, hexamethylene and normal hexane is 1: 1, and the volume fraction of isopropanol is 0.8%.
Preferably, the content of eluent used and ethyl acetate that ratio is 40 parts during step 4. eluting: 60 parts just oneself
Alkane, the aperture of filter membrane used is 0.22 μm.
The present invention uses vitamin D in Solid-Phase Extraction-high-efficient liquid phase chromatogram HPLC method detection health food3Content, changes
Tradition high-efficient liquid phase chromatogram HPLC method needs the method for positive-anti-phase dual system operation, improves pre-treatment time length, effectively becomes
Divide destructible, operator's technology required height, to problems such as Laboratory Instruments quantitative requirement are many so that vitamin D3Through soap
Directly cross Solid-Phase Extraction column purification after change, extraction, constant volume, enter reversed-phase HPLC-DAD liquid phase systems loading, in 5 minutes, go out peak, pole
The big time shortening experiment, improve the efficiency of experiment.It addition, by changing saponification temperature and saponification time so that sample
Product can saponification abundant, reduce impurity interference, improve the response rate of experiment.Therefore, disclosure satisfy that actual work by present invention mensuration
Need, filled up vitamin D in health food3The blank of content standard method, is to measure vitamin D in health food3Content
Quantitative approach efficient, effective.
Accompanying drawing explanation
Fig. 1 is the eluting effectiveness comparison figure of the eluent of different volumes ratio of the present invention；
Fig. 2 is the chromatogram of standard solution of the present invention；
Fig. 3 is the chromatogram of testing sample of the present invention；
Fig. 4 is the mark-on chromatogram of testing sample of the present invention.
Detailed description of the invention
One, instrument source explanation:
Agilent Technologies HPLC high performance liquid chromatograph (Agilent company of the U.S.)；
UV-detector (DAD) (Agilent company of the U.S.)；
Electronic balance (Mei Tele company of Switzerland)
Heating magnetic stirring apparatus (IKA company)；
Solid-phase extracting instrument (Beijing Zhuo Xin great achievement Science and Technology Ltd.)；
Rotary Evaporators (Asia, Shanghai Rong Shenghua company limited)；
Nitrogen evaporator (Tianjin Ao Tesaiensi Instrument Ltd.)；
Ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.).
Two, reagent source explanation:
Vitamin D3Standard substance (USP, lot number: POJ194)；
Methanol (high performance liquid chromatography is pure, U.S. Fisher Scientific, lot number: 114517)；
(high performance liquid chromatography is pure, Tianjin Kermel Chemical Reagent Co., Ltd., lot number: 20151013) for normal hexane；
(high performance liquid chromatography is pure, Tianjin Kermel Chemical Reagent Co., Ltd., lot number: 20130331) for ethyl acetate；
(high performance liquid chromatography is pure, Tianjin Kermel Chemical Reagent Co., Ltd., lot number: 20150309) for isopropanol；
(high performance liquid chromatography is pure, Tianjin Kermel Chemical Reagent Co., Ltd., lot number: 20150226) for dichloromethane；
Petroleum ether (analytical pure, Tianjin Zhi Yuan chemical reagent company limited, lot number: 2015122011)；
Potassium hydroxide (analytical pure, Tianjin Heng Xing chemical reagent Manufacturing Co., Ltd, lot number: 20160102)；
Ascorbic acid (analytical pure, Xilong Chemical Co., Ltd, lot number: 160102)；
Pyrogallic acid (analytical pure, Tianjin North Star great Zheng chemical reagent work, lot number: 20130615)；
Dehydrated alcohol (analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group, 20160107)；
Sodium chloride (analytical pure, Tianjin Zhi Yuan chemical reagent company limited, lot number: 20150201)；
2,6 ditertiary butyl p cresol (Chemical Reagent Co., Ltd., Sinopharm Group, lot number: F20080509)；
(lot number: 20160110, through 400 for analytical pure, Tianjin Kermel Chemical Reagent Co., Ltd. for anhydrous sodium sulfate
DEG C baking 4h)；
Ultra-pure water is prepared (Millipore company of the U.S.) by Milli-Q ultrapure water machine；
Silicagel column (Hangzhou Fu Yu science service company limited, 500mg/6mL).
Three, detecting step:
(1) preparation of standard solution
1., under the conditions of lucifuge, electronic balance is used accurately to weigh vitamin D3Standard substance, are configured to theoretical concentration with ethanol
Standard reserving solution for 1mg/mL.Using ethanol stepwise dilution during preparation, the reality calculating standard reserving solution by extension rate is dense
Degree, uses spectrophotometer be corrected and calculate correcting fluid actual concentrations under 264nm wavelength when calculating concentration.
2. draw above-mentioned standard reserving solution appropriate, use methanol dilution, compound concentration is 0.10 μ g/mL, 0.20 μ g/mL,
0.50 μ g/mL, 1.0 μ g/mL, 2.0 μ g/mL and the standard solution of 5.0 μ g/mL, and in the preservation of-20 DEG C of refrigerator.With standard series
Working solution concentration is abscissa, and peak area is that vertical coordinate draws standard curve.
(2) sample treatment
1. saponification: weigh the sample 10.0g to be detected of mix homogeneously, and be sequentially added into 1.5g ascorbic acid, 1.0g Jiao
Property gallic acid, 0.1g 2,6 ditertiary butyl p cresol, 100mL dehydrated alcohol, 35% potassium hydroxide aqueous solution 100mL, in temperature
Degree is condensing reflux 40 minutes on the heating magnetic stirring apparatus of 75 DEG C, is rapidly cooled to room temperature and obtains saponification liquor after taking-up.
Through test, the potassium hydroxide aqueous solution saponification effect of 10%, 20%, 30%, 40%, 50%, find to health care
Food vitamin D3In detection, 35% potassium hydroxide aqueous solution i.e. sponifiable is complete.In terms of saponification temperature test 50 DEG C, 60
DEG C, 70 DEG C, 80 DEG C, the saponification effect of 90 DEG C, find that, when saponification temperature is 75 DEG C, saponification 40 minutes i.e. sponifiable is complete, and quilt
Survey material will not be destroyed, need during less than this temperature to extend saponification time, easily make test substance aoxidize higher than this temperature.
2. extraction: be transferred in the separatory funnel of 500mL by saponification liquor, adds 100mL petroleum ether and extracts, and limit is shaken
Limit aerofluxus, stands after shaking 10 minutes and treats substantially to be layered, and upper strata is the petroleum ether dissolved with sample, is transferred to separately by lower floor's saponification liquor
Repeat above-mentioned extraction step 2 times after one separatory funnel, merge the petroleum ether of 3 times (more than 3 times can also) extraction gained, the most anhydrous
Sodium sulfate is sloughed except being collected in round-bottomed flask after trace water；Steam to closely at 45 DEG C in round-bottomed flask is put in Rotary Evaporators
Dry, dry up with Nitrogen evaporator after taking-up.
3. constant volume: washing the most a small amount of for the round-bottomed flask normal hexane dried up transfer are settled to 10mL volumetric flask
In stand-by.
4. purify: successively with dichloromethane and the normal hexane drip washing activated silica gel post of 5mL of 5mL, draw the sample after constant volume
Liquid 1.0mL transfers in silicagel column, then uses 5mL normal hexane successively, 5mL hexamethylene: normal hexane (1: 1) (by volume adds 0.8%
Isopropanol) (reason collecting liquid remove impurity using both different is that test substance will not be dissolved in mixed solution drip washing remove impurity
In the collection liquid that both is different), then add 5mL ethyl acetate: the mixed solution of normal hexane (40: 60) is by vitamin D3From silicon
Eluting collecting on glue post, then dries up with Nitrogen evaporator, adds 1.0mL methanol and dissolves, by 0.22 μm membrane filtration, treats HPLC
Measure.
Draw the sample liquid upper prop after constant volume, respectively test ethyl acetate and normal hexane mixed solution percentage 10: 90,20
: 80,30: 70,40: 60,50: 50,60: 40 collect as eluent, measure respectively and draw elution curve and see Fig. 1.Can by Fig. 1
Knowing, when ethyl acetate and normal hexane volume ratio are 40: 60, eluting rate is the highest, therefore selects ethyl acetate: normal hexane (40:
60) as eluent.
(3) high performance liquid chromatograph analysis
Filtrate step (2) obtained is injected high performance liquid chromatograph and is analyzed, and chromatographic condition is as follows:
Chromatographic column: HPLC SB C18 post (0.45 μm, 5mm × 150mm)；
Flowing phase: methanol+water (95+5)；
Flow velocity: 0.3mL/min；
Column temperature: 40 DEG C；
UV-detector (DAD) detection wavelength: 264nm；
Sample size is 5 μ L.
Four, the range of linearity and detection limit:
Under the conditions of lucifuge, preparation standard curve be 0.10 μ g/mL, 0.20 μ g/mL, 0.50 μ g/mL, 1.0 μ g/mL, 2.0 μ
g/mL、5.0μg/mL.Sample introduction 5 μ L, record chromatogram and peak area, equation of linear regression is y=46152x-1735.1, relevant
Coefficient is 0.9996.Finally being settled to 10mL by sampling 10.0g calculate, method detection is limited to 1.0 μ g/100g.Standard diagram is shown in
Fig. 2.
Five, recovery of standard addition and precision test:
Use sample to add standard substance mode, be added at three concentration levels, by above-mentioned sample treatment operating procedure
Carrying out 9 tests at different time, measurement result is as shown in the table:
When pitch-based sphere is 0.20～1.0mg/kg, the recovery of standard addition of this method is 87.8～105.8%, relatively marks
Quasi-deviation is 1.28～3.58, and sample collection of illustrative plates is shown in that Fig. 3, sample mark-on collection of illustrative plates are shown in Fig. 4.
When in experimentation due to deal with improperly emulsion occurs time, it is possible to use saturated nacl aqueous solution eliminates breast
Change；Water used in experimentation is ultra-pure water, is prepared by Milli-Q ultrapure water machine；Instrument after having tested uses super
Sound wave washer is carried out.
Claims (8)
1. a vitamin D3The detection method of content, is characterized in that step is as follows:
(1) preparation of standard solution
Vitamin D is accurately weighed under the conditions of lucifuge3Standard substance, are configured to, with ethanol, the standard inventory that theoretical concentration is 1mg/mL
Liquid；Draw above-mentioned standard reserving solution appropriate, use methanol dilution to be configured to the standard solution that concentration is 0.1～5.0 μ g/mL；
(2) sample treatment
1. saponification: weigh the sample to be detected of mix homogeneously, be sequentially added into ascorbic acid, pyrogallic acid, 2,6-bis-uncle
Butyl paracresol, dehydrated alcohol and potassium hydroxide aqueous solution, carry out saponification under the effect of heating magnetic stirring apparatus；
2. extraction: be transferred in separatory funnel by saponification liquor, adds extractant and extracts, merge the extractant of extraction gained,
It is collected in round-bottomed flask after removing trace water；Round-bottomed flask is steamed near dry, then dries up with Nitrogen evaporator；
3. constant volume: by washing the most a small amount of for the round-bottomed flask normal hexane dried up and be transferred in constant volume bottle stand-by；
4. purify: successively with dichloromethane and normal hexane drip washing activated silica gel post, draw the sample liquid after constant volume and transfer to silicagel column
In, dry up with Nitrogen evaporator after remove impurity, eluting, add methanol and dissolve, by obtaining filtrate after membrane filtration；
(3) high performance liquid chromatograph analysis
Filtrate step 4. obtained is injected high performance liquid chromatograph and is analyzed.
2. a vitamin D as claimed in claim 13The detection method of content, it is characterised in that chromatographic condition in step (3)
As follows:
Chromatographic column: HPLC SB C18 post (0.45 μm, 5mm × 150mm)；
Flowing phase: the methanol of 95% and the water of 5%；
Flow velocity 0.3mL/min；
Column temperature: 40 DEG C；
UV-detector (DAD) detection wavelength: 264nm；
Sample size is 5 μ L.
3. a vitamin D as claimed in claim 13The detection method of content, it is characterised in that preparation in described step (1)
During standard reserving solution use ethanol stepwise dilution, by extension rate calculate standard reserving solution actual concentrations, calculate concentration time
Spectrophotometer is used to be corrected and calculate correcting fluid actual concentrations under 264nm wavelength.
4. a vitamin D as claimed in claim 33The detection method of content, it is characterised in that described step 1. middle Vitamin C
Acid, pyrogallic acid, 2,6 ditertiary butyl p cresol are 1.5: 1: 0.1: 10 with the mass ratio of sample.
5. a vitamin D as claimed in claim 43The detection method of content, it is characterised in that described step 1. middle hydroxide
In aqueous solutions of potassium, the mass percent of potassium hydroxide is 35%, and saponification temperature is 75 DEG C, and saponification time is 40 minutes.
6. a vitamin D as claimed in claim 53The detection method of content, it is characterised in that described step 2. middle extractant
For petroleum ether, extraction times is more than 3 times.
7. a vitamin D as claimed in claim 63The detection method of content, it is characterised in that during the 4. remove impurity of described step first
Use normal hexane drip washing, then with hexamethylene, normal hexane and the mixed solution drip washing of isopropanol, hexamethylene and the volume of normal hexane
Ratio is 1: 1, and the volume fraction of isopropanol is 0.8%.
8. a vitamin D as claimed in claim 73The detection method of content, it is characterised in that described step 4. eluting time institute
By the content of eluent and ethyl acetate that ratio is 40 parts: the normal hexane of 60 parts, the aperture of filter membrane used is 0.22 μm.
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Cited By (4)
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| CN107703239A (en) * | 2017-11-14 | 2018-02-16 | 纽斯葆广赛（广东）生物科技股份有限公司 | A kind of assay method of soyabean protein powder vitamine D3 |
| CN109030648A (en) * | 2018-08-01 | 2018-12-18 | 北京出入境检验检疫局检验检疫技术中心 | The method and its sample-pretreating method of liposoluble vitamin content in a kind of detection formula milk |
| CN111579675A (en) * | 2020-05-28 | 2020-08-25 | 河南三方元泰检测技术有限公司 | Method for detecting fat-soluble vitamins in feed |
| CN113358795A (en) * | 2021-07-05 | 2021-09-07 | 诺安实力可商品检验(宁波)有限公司 | Liquid chromatography analysis method for determining vitamin D2 and vitamin D3 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107703239A (en) * | 2017-11-14 | 2018-02-16 | 纽斯葆广赛（广东）生物科技股份有限公司 | A kind of assay method of soyabean protein powder vitamine D3 |
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| CN111579675B (en) * | 2020-05-28 | 2024-02-02 | 山西海润牧大饲料有限公司 | Method for detecting fat-soluble vitamins in feed |
| CN113358795A (en) * | 2021-07-05 | 2021-09-07 | 诺安实力可商品检验(宁波)有限公司 | Liquid chromatography analysis method for determining vitamin D2 and vitamin D3 |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161207 |
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| RJ01 | Rejection of invention patent application after publication |