CN106442802B - A kind of method of eight chlorostyrenes in measurement milk - Google Patents
A kind of method of eight chlorostyrenes in measurement milk Download PDFInfo
- Publication number
- CN106442802B CN106442802B CN201611003613.6A CN201611003613A CN106442802B CN 106442802 B CN106442802 B CN 106442802B CN 201611003613 A CN201611003613 A CN 201611003613A CN 106442802 B CN106442802 B CN 106442802B
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- Prior art keywords
- acetonitrile
- milk
- sample
- chlorostyrenes
- aqueous solution
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Classifications
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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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/60—Construction of the column
Abstract
The present invention discloses a kind of method measuring eight chlorostyrenes in milk, and this method comprises the following steps：（1）The pretreatment of sample：Acetonitrile mechanical shaking extraction milk sample is first used, salt is then added into mixed liquor saltouts, and centrifuges, takes upper layer acetonitrile extracting solution；（2）Step（1）Acetonitrile extracting solution membrane filtration after, upper high performance liquid chromatograph is detected, Detection wavelength be 220 260nm, chromatographic column C18Column, mobile phase are the aqueous solution and acetonitrile of trifluoroacetic acid.This method sample treatment is simple, and organic solvent usage amount is few, meets the theory of Green Chemistry, and instrument and equipment requirement is relatively low, is suitble to promote and apply in base's detection department, the screening operation for eight chlorostyrene samples in great deal of milk sample.
Description
Technical field
The present invention relates to a kind of methods of eight chlorostyrenes in measurement milk.
Background technology
Eight chlorostyrenes CAS：29082-74-4;62601-62-1, molecular formula：C8Cl8, molecular weight：379.7096, English
Literary fame claims 1,2,3,4,5-pentachloro-6- (trichloroethenyl) benzene, is a kind of harmful hold
Long property organic pollution substance, is widely present in industrial products, more chlorinated aromatic compounds containing special construction are beautiful
Environmental Protection Agency of state is classified as one of the PBT substances of 12 kinds of I grades of priority acccess controls, can enter human body by the drinking-water and food chain of resident.
Milk is one of the main source that people obtain protein as a kind of high-protein food.It is currently continuous due to industrial pollution
Aggravation, there are a large amount of eight chlorostyrenes inside natural environment.It can be moved by eight chlorostyrene of the links such as herbage, drinking-water
It moves on to inside human body, and constantly gathers.In addition, eight chlorostyrenes may also be contained inside some packaging materials, when these
Packaging material be used for make contain milk box and bottle when, eight chlorostyrenes can penetrate into milk, further into
Enter in human body.The long-term accumulation of eight chlorostyrenes can cause serious injury to human body.Excessive eight chlorostyrene can cause slowly
Property poisoning, cause monster, tumour and immune function decline, and the most serious is reproductive system obstacles, cause the oligozoospermia of male,
Male degenerate so that male sterility it is occurred frequently.The women of child-bearing age are polluted by the substance for a long time, the fetal anomaly that can make to become pregnant can
Energy property greatly increases, and makes the face of fetus, the part deformity of limbs or sexual organ.In addition food chain amplification is penetrated with organism to turn
The substance after change may generate the ecosystem with our own health the lethality of bigger.And at present for this
The detection method research of substance it is seldom, in order to ensure numerous residents' milk safe for drinking, establish a kind of effectively simple measure
The method of eight chlorostyrenes is particularly important in milk.
Invention content
The technical problem to be solved by the present invention is to overcome the existing defects, provides eight chlorostyrenes in a kind of measurement milk
Method.
In order to solve the above technical problem, the present invention provides the following technical solutions：
The method of eight chlorostyrenes, includes the following steps in a kind of measurement milk：
（1）The pretreatment of sample：Acetonitrile mechanical shaking extraction milk sample is first used, salt is then added into mixed liquor carries out salt
Analysis, centrifugation, takes upper layer acetonitrile extracting solution；
（2）Step（1）Acetonitrile extracting solution membrane filtration after, upper high performance liquid chromatograph is detected, and Detection wavelength is
220-260nm, chromatographic column C18Column, mobile phase are the aqueous solution and acetonitrile of trifluoroacetic acid.
Preferably, step（1）Described in salt be sodium chloride and magnesium sulfate mixture.
It is highly preferred that the mass ratio of the sodium chloride and magnesium sulfate is 1:1.
When mechanical shaking extraction, the volume ratio of preferred milk sample and acetonitrile is 1:1.
When saltouing, salt is added into mixed liquor by a concentration of 0.05-0.15g/ml, the concentration of salt is preferably 0.1g/ml.
Preferably, step（2）Described in trifluoroacetic acid aqueous solution concentration of volume percent be 0.3%, pH value be 3~
4。
Preferably, step（2）Described in trifluoroacetic acid aqueous solution and acetonitrile volume ratio be 90:10.
Advantages of the present invention
This method sample treatment is simple, and organic solvent usage amount is few, meets the theory of Green Chemistry, and instrument and equipment requires phase
To relatively low, it is suitble to promote and apply in base's detection department, the screening operation for eight chlorostyrene samples in great deal of milk sample.
Description of the drawings
Attached drawing is used to provide further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the chromatogram of 100 μ g/L spiked levels；
Fig. 2 is the absorption curve of eight chlorostyrenes at different wavelengths.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
1, sample pre-treatments condition
5.0ml milk samples are measured, is fitted into 15ml tool plug centrifuge tubes, 5ml acetonitriles is added, vortex 30s is put into shaker
In, acutely vibrate 5min.0.5g sodium chloride and 0.5g anhydrous magnesium sulfates is added after completing in oscillation, then vibrates 5min.8000rpm
5min is centrifuged, after having centrifuged, upper layer acetonitrile extracting solution is drawn in another centrifuge tube with Dispette.With disposable note
Emitter draws 1-1.5ml extracting solutions, crosses in 0.22 μm of composite filter membrane filtering head to sample injection bottle, and upper machine measures.
2, instrument condition
High performance liquid chromatograph（waters2695）Two level array pipe detector, chromatographic column Xcharge C18 column
(250mm × 4.6mm, 5 μm, 100A), mobile phase are water and acetonitrile, water：Acetonitrile（v：V, 90:10）, wherein water contains 0.3%
Trifluoroacetic acid（v:v）, pH value is adjusted to 3-4 with concentrated ammonia liquor using preceding.Sampling volume is 20ul, and chromatographic column column temperature is 30 ± 5
℃。
3, the determination of maximum absorption wavelength
Set Detection wavelength as 200-400nm carry out field sweep experiment, the best Detection wavelength of optimization, as shown in Figure 2.It is real
Test the result shows that, 220-260nm have preferably absorb, wherein Detection wavelength be 233nm when, eight chlorine of target detection compound
Styrene has absorption maximum, and the sensitivity of detection method is best at this time.In the method, finally the wavelength of selected detector is
The chromatogram of 233nm, 100 μ g/L spiked levels are as shown in Figure 1.
4, the accuracy of method, precision and sensitivity
Eight chlorostyrene standard items are added into blank milk sample.After being handled using above-mentioned sample-pretreating method,
Upper machine measures, and measures the data such as recovery of standard addition, relative standard deviation, minimum detectability and minimum quantitative limit.The standard of this method
Exactness is embodied by recovery of standard addition, and it is 70-81% that mark-on experiment, which measures the rate of recovery,.Accuracy is by relative standard deviation（RSD）Come
It embodies, measures this method and 15% is less than to milk sample detection RSD.Sensitivity is embodied by minimum detectability and minimum quantitative limit.
Minimum detectability（LOD）It is calculated according to 3 times of to-noise ratios, minimum quantitative limit（LOQ）It is calculated according to 10 times of to-noise ratios：This method is most
Low detection limits are 10 μ g/ml, minimum to be quantitatively limited to 33 μ g/ml.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (5)
1. a kind of method measuring eight chlorostyrenes in milk, includes the following steps：
（1）The pretreatment of sample：Acetonitrile mechanical shaking extraction milk sample is first used, salt is then added into mixed liquor saltouts, from
The heart takes upper layer acetonitrile extracting solution；
（2）Step（1）Acetonitrile extracting solution membrane filtration after, upper high performance liquid chromatograph-two level array pipe detector is examined
It surveys, Detection wavelength 220-260nm, chromatographic column C18Column, mobile phase are the aqueous solution and acetonitrile of trifluoroacetic acid, the trifluoro second
The aqueous solution of acid and the volume ratio of acetonitrile are 90:10.
2. according to the method described in claim 1, it is characterized in that：Step（1）Described in salt be the mixed of sodium chloride and magnesium sulfate
Close object.
3. according to the method described in claim 2, it is characterized in that：The mass ratio of the sodium chloride and magnesium sulfate is 1:1.
4. according to the method described in claim 1, it is characterized in that：Step（2）Described in Detection wavelength be 233nm.
5. according to the method described in claim 1, it is characterized in that：Step（2）Described in trifluoroacetic acid aqueous solution volume
Percent concentration is 0.3%, and pH value is 3~4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611003613.6A CN106442802B (en) | 2016-11-15 | 2016-11-15 | A kind of method of eight chlorostyrenes in measurement milk |
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| CN201611003613.6A CN106442802B (en) | 2016-11-15 | 2016-11-15 | A kind of method of eight chlorostyrenes in measurement milk |
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| Publication Number | Publication Date |
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| CN106442802A CN106442802A (en) | 2017-02-22 |
| CN106442802B true CN106442802B (en) | 2018-10-12 |
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| JP2002355079A (en) * | 2001-03-14 | 2002-12-10 | Takara Bio Inc | Method for detecting endocrine disruptor |
| US9408866B2 (en) * | 2012-04-26 | 2016-08-09 | Niva | Method for detoxification or measurement of at least one compound or at least one fluid in a host body |
| CN103399108B (en) * | 2013-08-16 | 2015-07-15 | 光明乳业股份有限公司 | Pretreatment method and ciprofloxacin and erythromycin detection method |
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