CN104330510B - A kind of method of alkyl phenol and its ethers in quick detection tissue - Google Patents
A kind of method of alkyl phenol and its ethers in quick detection tissue Download PDFInfo
- Publication number
- CN104330510B CN104330510B CN201410534866.0A CN201410534866A CN104330510B CN 104330510 B CN104330510 B CN 104330510B CN 201410534866 A CN201410534866 A CN 201410534866A CN 104330510 B CN104330510 B CN 104330510B
- Authority
- CN
- China
- Prior art keywords
- alkyl phenol
- ethers
- sample
- phenol
- tissue
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of method for detecting alkyl phenol and its ethers content in tissue, tissue sample is shredded into 5mm × 5mm sizes first, weigh 0.5 1.5g, add more than 5mL methyl alcohol, 30 100 DEG C of more than ultrasonic extraction 15min, extract solution nitrogen is blown near dry, methanol constant volume, again through 0.22 μm of membrane filtration after, using liquid chromatography tandem mass spectrometry test and analyze；Finally according to the content of alkyl phenol and its ethers in the sample liquid for analyzing, you can converse alkyl phenol and its ethers content in tissue sample.Present invention optimizes extraction mode and extraction conditions, the test condition of instrument, liquid chromatogram separation, the electro-spray ionization monitoring technology of APES in tissue are established.The method is easy to operate, quick, and test limit is low, and the rate of recovery is high, is the Perfected process of alkyl phenol and APES in quick detection tissue.
Description
Technical field
The invention belongs to compound test technical field.More particularly, to alkyl phenol in a kind of quick detection tissue
And its method for ethers.
Background technology
APES（APEO）It is to be formed through catalysis by alkyl phenol and oxirane.APES
It is another major class nonionic surface active agent after AEO, the whole world is per annual consumption more than 400,000
Ton, wherein with NPE（NPEO）At most, 80%-85%, OPEO are accounted for（OPEO）Account for 15% with
On.APES is used as the removing that digesting assistant promotes lignin and resin in paper industry, improves paper pulp and receives
Rate；Ink is sloughed in floatation as deinking agent；As formulation for coating material etc..
APES belongs to incretion interferent, even if quantity is few, can also allow organism endocrine imbalance,
There are a variety of anomalies.In recent years, APES（APEOs）And its metabolite alkyl phenol is strong to human body
Therefore the harm of health and ecological environment to it is widely known that must strengthen monitoring and detect.European Union's paper for daily use nascent state mark
Label method（2009/568/EC）Regulation：When paper for daily use uses chemicals in process of production, should avoid using hostile environment and be good for
The APES of health.
The detection method of APES reported at present, primarily directed to fields such as water body, food, for
The assay method of APES and its catabolite alkyl phenol in tissue, less report.And it is directed to different samples
The problems such as product, the foundation of its detection method, influence factor and detection efficiency, be all entirely different, therefore, set up a kind of energy
The method of APES and its catabolite alkyl phenol is significant in enough quick detection tissues.
The content of the invention
The technical problem to be solved in the present invention is to overcome the shortcomings of alkyl phenol and its ethers detection technique in existing tissue,
A kind of ultrasonic extraction combination liquid chromatography-tandem mass spectrometry is provided（LC-MS/MS）Quick detection tissue in alkyl phenol and its ether
The method of class.
It is an object of the invention to provide a kind of method of alkyl phenol and its ethers in quick detection tissue.
Another object of the present invention is to provide the application of methods described.
Above-mentioned purpose of the present invention is achieved through the following technical solutions：
The invention discloses a kind of method for detecting alkyl phenol and its ethers content in tissue, comprise the following steps：
S1. sample treatment
S11. tissue sample is shredded, adds methyl alcohol, carry out ultrasonic extraction, obtain extract solution；
S12. extract solution nitrogen is blown to closely do, through 0.22 μm of membrane filtration after methanol constant volume；
S2. Liquid Chromatography-Tandem Mass Spectrometry detection and analysis；
S3. result is calculated：Contained according to alkyl phenol and its ethers in the sample liquid that Liquid Chromatography-Tandem Mass Spectrometry is tested and analyzed
Amount, converses alkyl phenol and its ethers content in tissue sample.
Wherein preferably, step S11 is that tissue sample is shredded into 5mm × 5mm sizes, weighs 0.5-1.5g, is added
More than 5mL methyl alcohol, more than 30-100 DEG C of ultrasonic extraction 15min.
Preferably, the addition of methyl alcohol described in step S11 is 15-30mL.
Preferably, the time of ultrasonic extraction described in step S11 is more than 60-90min.
Preferably, extracted described in step S11 and repeated 3-5 times, merge extract solution.
Preferably, step S11 is that tissue sample is shredded into 5mm × 5mm sizes, weighs 1g, adds 15mL methyl alcohol, 40
DEG C ultrasonic extraction 60min, repeats to extract 3 times, merges extract solution；
Preferably, step S12 is that extract solution nitrogen is blown near dry, methanol constant volume to 1mL, through 0.22 μm of filter of organic system
Membrane filtration.
Alkyl phenol and its ethers content are calculated as follows in tissue sample described in step S3：
X = （C·V·1000）/（m·1000）；
In formula：X is the content of alkyl phenol and its ethers in sample, and unit is mg/kg；
C is the content of alkyl phenol and its ethers in sample liquid, and unit is mg/L；
V is the final constant volume of sample liquid, and unit is mL；
M is the sample size representated by final sample liquid, and unit is g.
In addition, the above method is in alkyl phenol in detecting tissue and its application in ethers content also early protection of the invention
Within the scope of.
Extraction mode and extraction conditions, the test condition of instrument present invention optimizes sample, establish alkane in tissue
The liquid chromatogram of base phenol polyethenoxy ether is separated, electro-spray ionization monitoring technology.Mode using ultrasonic extraction is entered to paper product
Row extraction, is optimized to extraction volume, extraction temperature and time etc., has reached good effect of extracting, to final detection
The effect of the detection such as limit and the rate of recovery serves vital effect.
Those skilled in the art's common knowledge, for different detection objects, different detection architectures, each of which link and every
One reagent has very big influence to testing result.Therefore, for different detection objects, extraction mode, extract, color
Spectrum testing conditions etc. must all reach an optimal unified integrality, can be only achieved best Detection results.
Even if paper and textile are equally fiber substances, but its detection method is also different, article《HPLC methods are surveyed
Determine AP and APEO in textile》In（212.1）When specifically disclosing use methyl alcohol as extractant, effect of extracting is taken out with Soxhlet
Formulation is optimal, and microwave-assisted is slightly worse, and ultrasonic extraction method is worst.But, for paper of the invention, using methyl alcohol as
In conjunction with the method for ultrasonic extraction, testing result is but optimal to extract solution.This result also substantially demonstrate different samples for
The differentia influence of testing result.The present invention is had been surprisingly found that based on this, using methyl alcohol as extract solution, using the side of ultrasonic extraction
Formula, extracts to APES in tissue and alkyl phenol, further combined with Liquid Chromatography-Tandem Mass Spectrometry,
The analysis method of quick detection alkyl phenol and its ethers is established, recovery of standard addition can reach the level higher than 100%, and method
It is reproducible.
In addition, the process conditions tested and analyzed for specific Liquid Chromatography-Tandem Mass Spectrometry, in order to reach preferably inspection
Effect is surveyed, can be adjusted according to different detection materials, with octyl phenol, nonyl phenol, OPEO and nonyl
As a example by phenol polyethenoxy ether：
（1）The optimal chromatographic retention of octyl phenol, nonyl phenol, OPEO and NPE
Respectively 3.15min, 3.61min, 3.34min, 3.92min.
（2）The liquid phase chromatogram condition of the alkyl phenol such as octyl phenol or nonyl phenol：
Chromatographic column：Waters Symmetry Shieldtm RP18,5 μm, 4.6 × 150mm；
Mobile phase：0.1% aqueous formic acid（A）, methyl alcohol（B）, flow phase composition and be shown in Table 1；
Flow：1mL/min；
Column temperature：40℃；
Sample size：10μL.
Table 1 flows phase composition
（3）The Mass Spectrometry Conditions of the alkyl phenol such as octyl phenol or nonyl phenol：
a）Ionization mode：Electro-spray ionization；
b）Check system：Using negative ion mode；
c）Ion source temperature（TEM）：550℃；
d）Mass scan range：100m/z-250m/z；
e）Selection monitoring ion：m/z 205（OP）, m/z 219（NP）；
f）Atomizer, collision gas：High pure nitrogen；
g）Gas curtain atmospheric pressure（CUR）：20psi；
h）Atomization gas pressure（GS1）：55 psi；
i）Secondary air speed（GS2）：50 psi；
j）Collision gas（CAD）：5 psi；
（4）The liquid chromatogram bar of the APES such as OPEO or NPE
Part：
Chromatographic column：Waters Symmetry Shieldtm RP18,5 μm, 4.6 × 150mm；Mobile phase：0.1% formic acid water
Solution（A）, methyl alcohol（B）, flow phase composition and be shown in Table 2；Flow：1mL/min；Column temperature：35℃；Sample size：10μL.
Table 2 flows phase composition
（5）The liquid chromatogram bar of the APES such as OPEO or NPE
Part：
a）Ionization mode：Electro-spray ionization；
b）Check system：Using positive ion mode；
c）Ion source temperature（TEM）：550℃；
d）Mass scan range：150m/z-1000m/z；
e）Selection detection ion：m/z 361.5+Δ44（OPEO, n=3~16）, m/z 375.5+Δ44（NPEO,n=3
~16）；
f）Atomizer, collision gas：High pure nitrogen；
g）Gas curtain atmospheric pressure（CUR）：20psi；
h）Atomization gas pressure（GS1）：55 psi；
i）Secondary air speed（GS2）：50 psi；
j）Collision gas（CAD）：5 psi；
The invention has the advantages that：
The invention discloses a kind of ultrasonic extraction combination Liquid Chromatography-Tandem Mass Spectrometry（LC-MS/MS）Quick detection paper handkerchief
The method of alkyl phenol and its ethers content in paper, has broken inclined as extract solution carries out the worst technology of ultrasonic extraction effect with methyl alcohol
See, tissue sample is shredded into 5mm × 5mm sizes first, weigh 0.5-1.5g, add more than 5mL methyl alcohol, 30-100 DEG C surpasses
Sound extracts more than 15min, and extract solution nitrogen is blown near dry, methanol constant volume, then through 0.22 μm of membrane filtration after, using liquid phase color
Spectrum-tandem mass spectrometry is tested and analyzed；Finally according to the content of alkyl phenol and its ethers in the sample liquid for analyzing, you can conversion paper delivery
Alkyl phenol and its ethers content in towel pattern product.
Present invention optimizes ultrasonic extraction mode and extraction conditions, the test condition of instrument, alkyl in tissue is established
The liquid chromatogram of phenol polyethenoxy ether is separated, electro-spray ionization monitoring technology.The method is easy to operate, quick, and test limit is low,
The rate of recovery is high, is the Perfected process of alkyl phenol and APES in quick detection tissue.
Brief description of the drawings
Fig. 1 is the chromatogram of standard items octyl phenol and nonyl phenol.
Fig. 2 is standard items OPEO and NPE chromatogram.
Fig. 3 is the influence for extracting volume to the rate of recovery.
Fig. 4 is influence of the extraction temperature to the rate of recovery.
Fig. 5 is influence of the extraction time to the rate of recovery.
Specific embodiment
The present invention, but embodiment are further illustrated below in conjunction with Figure of description and specific embodiment not to the present invention
Limit in any form.Unless stated otherwise, reagent, the method and apparatus that the present invention is used are for the art is routinely tried
Agent, method and apparatus.Unless stated otherwise, following examples agents useful for same and material are purchased in market.
Following examples instrument：The series type high performance liquid chromatographs of Agilent Technologies 1200
（Agilent companies of the U.S.）, API3200 LC-MS/MS System mass spectrographs（American AB SCIENCE companies）, AS7240B types
Ultrasonic cleaner（AUTO Science）.
Following examples agents useful for same：OPEO OPnEO（CAS：9002-93-1, polymerization degree n=9-10,
CHEM SERVICE companies of the U.S.）；NPE NPnEO（CAS：9016-45-9, polymerization degree n=9-10, the U.S.
CHEM SERVICE companies）；Octyl phenol OP（CAS：140-66-9, purity 99.0%, German Dr. Ehrenstorfer companies）；
Nonyl phenol NP（CAS：25154-52-3, purity 100%, German Dr. Ehrenstorfer companies）；Methyl alcohol（Chromatographically pure, Germany
Merck companies）；Ammonium acetate（10mmol/L）；Aqueous formic acid（Concentration 0.1%）；Ultra-pure water is by French Milli-Q System
（0.22 μm of filter membrane）It is obtained.
The Liquid Chromatography-Tandem Mass Spectrometry testing conditions of embodiment 1
The present embodiment by taking octyl phenol, nonyl phenol, OPEO and NPE standard items as an example,
Carry out Liquid Chromatography-Tandem Mass Spectrometry detection and analysis.
1st, the optimal chromatographic retention of octyl phenol, nonyl phenol, OPEO and NPE
Respectively 3.15min, 3.61min, 3.34min, 3.92min.
2nd, the liquid phase chromatogram condition of the alkyl phenol such as octyl phenol or nonyl phenol：
Chromatographic column：Waters Symmetry Shieldtm RP18,5 μm, 4.6 × 150mm；
Mobile phase：Methyl alcohol（A）, ammonium acetate（B）, flow phase composition and be shown in Table 1；
Flow：1mL/min；
Column temperature：40℃；
Sample size：10μL.
Table 1 flows phase composition
3rd, the Mass Spectrometry Conditions of the alkyl phenol such as octyl phenol or nonyl phenol：
a）Ionization mode：Electro-spray ionization；
b）Check system：Using negative ion mode；
c）Ion source temperature（TEM）：550℃；
d）Mass scan range：200m/z-225m/z；
e）Selection monitoring ion：m/z 205（OP）, m/z 219（NP）；
f）Atomizer, collision gas：High pure nitrogen；
g）Gas curtain atmospheric pressure（CUR）：20psi；
h）Atomization gas pressure（GS1）：55 psi；
i）Secondary air speed（GS2）：50 psi；
j）Collision gas（CAD）：5 psi；
4th, the liquid phase chromatogram condition of the APES such as OPEO or NPE：
Chromatographic column：Waters Symmetry Shieldtm RP18,5 μm, 4.6 × 150mm；Mobile phase：0.1% formic acid water
Solution（A）, methyl alcohol（B）, flow phase composition and be shown in Table 2；Flow：1mL/min；Column temperature：35℃；Sample size：10μL.
Table 2 flows phase composition
5th, the liquid phase chromatogram condition of the APES such as OPEO or NPE：
a）Ionization mode：Electro-spray ionization；
b）Check system：Using positive ion mode；
c）Ion source temperature（TEM）：550℃；
d）Mass scan range：150m/z-1000m/z；
e）Selection monitoring ion：m/z 361.5+Δ44（OPEO, n=3~16）, m/z 375.5+Δ44（NPEO,n=3
~16）；
f）Atomizer, collision gas：High pure nitrogen；
g）Gas curtain atmospheric pressure（CUR）：20psi；
h）Atomization gas pressure（GS1）：55 psi；
i）Secondary air speed（GS2）：50 psi；
j）Collision gas（CAD）：5 psi；
6th, chromatogram and chromatographic retention
（1）The chromatogram difference of standard items octyl phenol, nonyl phenol, OPEO and NPE
As shown in Figures 1 and 2.
The chromatographic retention of octyl phenol, nonyl phenol, the OPEO and NPE such as institute of table 3
Show.
Each material chromatographic retention of table 3
7th, result is calculated
Alkyl phenol and its ethers content are calculated as follows in tissue sample：
X = （C·V·1000）/（m·1000）；
In formula：X is the content of alkyl phenol and its ethers in sample, and unit is mg/kg；
C is the content of alkyl phenol and its ethers in sample liquid, and unit is mg/L；
V is the final constant volume of sample liquid, and unit is mL；
M is the sample size representated by final sample liquid, and unit is g.
The optimization of the tissue sample treatment of embodiment 2 and extraction conditions
The present embodiment is with liquid chromatography-tandem mass spectrometry same as Example 1（LC-MS/MS）Condition, to sample treatment and
Extraction conditions is optimized.
1st, the optimization of volume is extracted
Tissue sample is shredded（5mm×5mm）, weigh about 1g samples, be separately added into 5,10,15,20,30,50mL first
Alcohol, ultrasonic extraction 3 times, each extraction time is 60min, and extraction temperature is 40 DEG C, merges extract solution, and nitrogen is blown near dry, first
Alcohol is settled to 1mL, through 0.22 μm of membrane filtration of organic system, carries out Liquid Chromatography-Tandem Mass Spectrometry detection and analysis.Test result is such as
Shown in accompanying drawing 3.
It can be seen that influence of the extraction volume to the rate of recovery is larger, and when volume is extracted more than 15mL, the rate of recovery
It is higher.
2nd, the optimization of extraction temperature
Tissue sample is shredded（5mm×5mm）, about 1g samples, plus 15mL methyl alcohol are weighed, ultrasonic extraction 3 times extracts every time
The time is taken for 60min, extraction temperature is 30,40,50,80,100 DEG C of merging extract solutions, nitrogen is blown to closely do, and methanol constant volume is extremely
1mL, through 0.22 μm of membrane filtration of organic system, carries out Liquid Chromatography-Tandem Mass Spectrometry detection and analysis.The test result such as institute of accompanying drawing 4
Show.
It can be seen that influence of the extraction temperature to the rate of recovery is less, when 30 DEG C -100 DEG C of extraction temperature, reclaim
Rate is all higher than 92%.
3rd, the optimization of extraction time
Tissue sample is shredded（5mm×5mm）, about 1g samples, plus 15mL methyl alcohol are weighed, ultrasonic extraction 3 times extracts every time
Take the time for 15,30,60,90,120,240min, extraction temperature is 40 DEG C, merges extract solution, and nitrogen is blown near dry, and methyl alcohol is fixed
Hold to 1mL, through 0.22 μm of membrane filtration of organic system, carry out Liquid Chromatography-Tandem Mass Spectrometry detection and analysis.Test result such as accompanying drawing
Shown in 5.
It can be seen that influence of the extraction time to the rate of recovery is larger, when extraction time is more than 60min, reclaim
Rate is higher.
In sum, running cost, detection time etc. factor are considered further that, finally determines that optimal extraction conditions is：
Tissue sample is shredded into 5mm × 5mm sizes, 1g is weighed, adds 15mL methyl alcohol, 40 DEG C of ultrasonic extraction 60min to repeat to extract
3 times, merge extract solution；Extract solution nitrogen is blown near dry, methanol constant volume to 1mL, through 0.22 μm of membrane filtration of organic system.
The range of linearity of embodiment 3, detection limit and lower limit of quantitation
Octyl phenol and nonyl phenol, OPEO and NPE are made into a series of quality respectively
The mixed standard solution sample introduction of concentration, draws standard curve, with the lower limit of quantitation that signal to noise ratio is each material of 10 calculating（LOQ）.Line
Property equation and detection limit are as shown in table 4.
The linear equation of table 4, detection limit and lower limit of quantitation
The rate of recovery and precision of the inventive method of embodiment 4
1st, the standard liquid of various concentrations is added in the tissue without object, recovery of standard addition and precision is carried out
Experiment, mark-on sample is detected.
2nd, mark-on tissue sample is shredded into 5mm × 5mm sizes, weighs 1g, add 15mL methyl alcohol, 40 DEG C of ultrasonic extractions
60min, repeats to extract 3 times, merges extract solution；Extract solution nitrogen is blown near dry, methanol constant volume to 1mL, through organic system
0.22 μm of membrane filtration.
3rd, Liquid Chromatography-Tandem Mass Spectrometry detection and analysis.Two average recovery rates of pitch-based sphere（Each addition concentration is put down
Row is determined 6 times）It is as shown in table 5 with precision result.
The recovery of standard addition of table 5 and precision result
Result shows, octyl phenol and nonyl phenol, OPEO and Nonyl pheno in tissue sample
The rate of recovery of ether has all reached more than 90% substantially.Wherein, the rate of recovery of nonyl phenol and NPE is even more and reaches
Level higher than 100%.
Meanwhile, very well, method is reproducible for the result precision of detection method.
The detection of the tissue sample of embodiment 5
Have selected the paper handkerchief magma of the different brand of kind more than 60, tissue and detected that method is ibid.
Result such as table 6, white 7 and table 8 shown in.
The sample tests of table 6
The sample tests of table 7
The sample tests of table 8
Result shows, main detection material is NPE, and detected level is between 5.3-88.1mg/kg, bad
Recall rate is higher in matter paper, is not detected in paper magma.This also show in the market paper for daily use useization in process of production
During product, it is possible to the materials such as the APES of hostile environment and health can be brought into, related paper product should be caused to produce
The concern of enterprise.
Comparative example
1st, in the method for the invention, the pre-treating method of sample it is critical that a step, specific ultrasonic extraction
Method and condition, the effect to detections such as final detection limit and the rate of recovery serve vital effect.
The liquid chromatography-tandem mass spectrometry inspection of the optimal extracting process of sample pre-treatments, embodiment 1 that determine according to embodiment 2
Survey condition, respectively to octyl phenol, nonyl phenol, OPEO and NPE in mark-on tissue sample
Detected.
（1）Experimental group：Tissue sample is shredded into 5mm × 5mm sizes, 1g is weighed, 15mL methyl alcohol, 40 DEG C of ultrasounds is added
Extraction 60min, repeats to extract 3 times, merges extract solution；Extract solution nitrogen is blown near dry, methanol constant volume to 1mL, through organic
It is that LC-MS/MS is analyzed after 0.22 μm of membrane filtration.
The operating condition of following contrast groups is with experimental group difference：
（2）Contrast groups 1：Ultrasonic extraction is with ethyl acetate as extract.
（3）Contrast groups 2：Ultrasonic extraction is with dichloromethane as extract.
2nd, result
Testing result is as shown in table 9.
Table 9
Claims (2)
1. it is a kind of detect tissue in alkyl phenol and its ethers content method, it is characterised in that comprise the following steps：
S1. sample treatment
S11. tissue sample is shredded into 5mm × 5mm sizes, weighs 1g, add 15mL methyl alcohol, 40 DEG C of ultrasonic extraction 60min
Extract solution is obtained, is repeated 3 times, merge extract solution；
S12. extract solution nitrogen is blown to closely do, after methanol constant volume to 1mL, through 0.22 μm of membrane filtration of organic system；
S2. Liquid Chromatography-Tandem Mass Spectrometry detection and analysis；
S3. result is calculated：According to the content of alkyl phenol and its ethers in the sample liquid that Liquid Chromatography-Tandem Mass Spectrometry is tested and analyzed,
Converse alkyl phenol and its ethers content in tissue sample；
Wherein, alkyl phenol and its ethers content are calculated as follows in tissue sample described in step S3：
X = （C·V·1000）/（m·1000）；
In formula：X is the content of alkyl phenol and its ethers in sample, and unit is mg/kg；
C is the content of alkyl phenol and its ethers in sample liquid, and unit is mg/L；
V is the final constant volume of sample liquid, and unit is mL；
M is the sample size representated by final sample liquid, and unit is g；
Wherein, the condition of Liquid Chromatography-Tandem Mass Spectrometry detection and analysis is as follows described in step S2：
（1）When the alkyl phenol and its ethers are octyl phenol, nonyl phenol, OPEO and NPE
When, chromatographic retention is respectively 3.15min, 3.61min, 3.34min, 3.92min；
（2）When the alkyl phenol and its ethers are the alkyl phenols such as octyl phenol or nonyl phenol, liquid phase chromatogram condition：
Chromatographic column：Waters Symmetry Shieldtm RP18,5 μm, 4.6 × 150mm；
Mobile phase：0.1% aqueous formic acid（A）, methyl alcohol（B）, flow the following table of phase composition；
Flow：1mL/min；
Column temperature：40℃；
Sample size：10μL；
（3）When the alkyl phenol and its ethers are the alkyl phenols such as octyl phenol or nonyl phenol, Mass Spectrometry Conditions：
a）Ionization mode：Electro-spray ionization；
b）Check system：Using negative ion mode；
c）Ion source temperature（TEM）：550℃；
d）Mass scan range：100m/z-250m/z；
e）Selection monitoring ion：m/z 205（OP）, m/z 219（NP）；
f）Atomizer, collision gas：High pure nitrogen；
g）Gas curtain atmospheric pressure（CUR）：20psi；
h）Atomization gas pressure（GS1）：55 psi；
i）Secondary air speed（GS2）：50 psi；
j）Collision gas（CAD）：5 psi；
（4）When the alkyl phenol and its ethers are the alkyl phenol polyoxy second such as OPEO or NPE
During alkene ether, liquid phase chromatogram condition：
Chromatographic column：Waters Symmetry Shieldtm RP18,5 μm, 4.6 × 150mm；
Mobile phase：0.1% aqueous formic acid（A）, methyl alcohol（B）, flow the following table of phase composition；
Flow：1mL/min；
Column temperature：35℃；
Sample size：10μL；
（5）When the alkyl phenol and its ethers are the alkyl phenol polyoxy second such as OPEO or NPE
During alkene ether, liquid phase chromatogram condition：
a）Ionization mode：Electro-spray ionization；
b）Check system：Using positive ion mode；
c）Ion source temperature（TEM）：550℃；
d）Mass scan range：150m/z-1000m/z；
e）Selection detection ion：m/z 361.5+Δ44（OPEO, n=3~16）, m/z 375.5+Δ44（NPEO, n=3~
16）；
f）Atomizer, collision gas：High pure nitrogen；
g）Gas curtain atmospheric pressure（CUR）：20psi；
h）Atomization gas pressure（GS1）：55 psi；
i）Secondary air speed（GS2）：50 psi；
j）Collision gas（CAD）：5 psi.
2. claim 1 methods described is in alkyl phenol in detecting tissue and its application in ethers content.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410534866.0A CN104330510B (en) | 2014-10-11 | 2014-10-11 | A kind of method of alkyl phenol and its ethers in quick detection tissue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410534866.0A CN104330510B (en) | 2014-10-11 | 2014-10-11 | A kind of method of alkyl phenol and its ethers in quick detection tissue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104330510A CN104330510A (en) | 2015-02-04 |
| CN104330510B true CN104330510B (en) | 2017-07-11 |
Family
ID=52405278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410534866.0A Expired - Fee Related CN104330510B (en) | 2014-10-11 | 2014-10-11 | A kind of method of alkyl phenol and its ethers in quick detection tissue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104330510B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699571B (en) * | 2016-03-18 | 2017-12-15 | 中华人民共和国鄞州出入境检验检疫局 | Assay method of the short chain to tert-octylphenol ethoxylate in a kind of textile |
| CN106950295A (en) * | 2017-02-27 | 2017-07-14 | 华南理工大学 | A kind of method of high hydroscopic resin remaining propylene acid in Accurate Determining amenities |
| WO2020110584A1 (en) * | 2018-11-28 | 2020-06-04 | 株式会社島津製作所 | Method for analyzing azo compound |
| WO2020110583A1 (en) * | 2018-11-29 | 2020-06-04 | 株式会社島津製作所 | Toxic substance analysis system and program for toxic substance analysis |
| CN109884208A (en) * | 2019-03-18 | 2019-06-14 | 珠海格力电器股份有限公司 | Method for detecting 4-nonylphenol ethoxylate by using ultra-high performance liquid chromatography-PDA (personal digital Assistant) |
| CN110045043A (en) * | 2019-05-22 | 2019-07-23 | 珠海格力电器股份有限公司 | Method for determining content of 4-nonyl phenol and/or 4-nonyl phenol ethoxy compound |
| CN114894930B (en) * | 2022-04-28 | 2023-10-20 | 浙江师范大学 | Method for detecting alkylphenol ethoxylate content in textile by high performance liquid chromatography |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013231711A (en) * | 2012-04-02 | 2013-11-14 | Hitachi High-Technologies Corp | Method of analyzing volatile substance included in sample liquid |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120270205A1 (en) * | 2011-04-19 | 2012-10-25 | Patel Sanjay V | High-flux chemical sensors |
-
2014
- 2014-10-11 CN CN201410534866.0A patent/CN104330510B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013231711A (en) * | 2012-04-02 | 2013-11-14 | Hitachi High-Technologies Corp | Method of analyzing volatile substance included in sample liquid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104330510A (en) | 2015-02-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104330510B (en) | A kind of method of alkyl phenol and its ethers in quick detection tissue | |
| CN107907614A (en) | A kind of molecular engram solid phase extraction high performance liquid chromatography tandem mass spectrum assay method of bisphenol compound | |
| CN102183606B (en) | Method for detecting estrogen, nonyl phenol, octyl phenol and bisphenol A in water body sediment together | |
| CN103529153B (en) | Common rapid detection method for various pesticide residues in soybeans | |
| WO2021159889A1 (en) | Detection method based on supercritical fluid chromatography and ionic liquid post-column addition reaction | |
| CN101661021B (en) | Method for detecting content of bisphenol A | |
| CN104483427A (en) | Method for separating, enriching and detecting 12 antibiotics in drinking water source | |
| CN102207495A (en) | Method for determining content of glyphosate in soils by using high performance liquid chromatography method | |
| CN111474266B (en) | Method for detecting phenolic compounds in water | |
| CN102662020A (en) | GC-MS detection method for phosphate ester flame retardant plasticizers in textiles | |
| CN105259287A (en) | Second-order mass spectrometric detection method for bisphenol substances in water environment | |
| CN104133017A (en) | Determination method for content of polyoxyethylene octylphenol ether and polyoxyethylene nonyl phenyl ether in water-based adhesive | |
| CN103728398B (en) | A kind of Ion-pair Liquid Chromatography measures the method for dyeing and finishing auxiliaries for textile neutral line alkyl benzene sulfonate | |
| CN108872412A (en) | QuEChERS method based on graphene establishes the UPLC-MS/MS detection method of fat-soluble saxitoxin | |
| CN103235081A (en) | Method for measuring phenolic compounds in textiles and leather products | |
| CN103293260B (en) | Method for high-efficiency detection of rhodamine B in food and rapid detection kit | |
| CN113533548B (en) | Method for detecting 1-vinyl imidazole in chemical product | |
| CN101644697A (en) | Detection method of IPBC in cosmetics | |
| CN108760920A (en) | A method of cyazofamid and its metabolite residue amount are measured based on HPLC-MSMS methods | |
| CN102706981B (en) | Method for quantitatively analyzing hydrogen peroxide working solution produced by anthraquinone process by using normal-phase efficient liquid adsorption chromatography | |
| CN103808822A (en) | LC-QTOF (Liquid Chromatography-Quadrupole Time Of Flight) analysis method for distinguishing resveratrol of different resources | |
| CN108414460B (en) | Method for determining content of cannabidiol based on silver nano ultraviolet-visible spectrophotometry | |
| CN109374790A (en) | A kind of α-ketoglutaric acid assay kit and method based on HPLC | |
| Wang et al. | Application of cloud point methodology to the determination of nitroanilines in natural water | |
| CN103630625A (en) | Detection method for alkylphenol polyoxyethylene ether in washing product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170711 Termination date: 20171011 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |