CN103630625A - Detection method for alkylphenol polyoxyethylene ether in washing product - Google Patents
Detection method for alkylphenol polyoxyethylene ether in washing product Download PDFInfo
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Abstract
The invention relates to a detection method for alkylphenol polyoxyethylene ether in a washing product. The detection method comprises the steps of: firstly, respectively preparing alkylphenol polyoxyethylene ether standard product solutions with different concentrations and washing product solutions with different concentrations and not containing alkylphenol polyoxyethylene ether, namely, blank sample solutions; secondly, preparing a washing product sample solution, then carrying out qualitative and quantitative analysis on the alkylphenol polyoxyethylene ether standard product solutions, a comparison product solution and the washing product sample solution by adopting a liquid chromatogram system to inspect a linear relation, a recovery rate and a precision degree of the method; finally, measuring the content of alkylphenol polyoxyethylene ether in the washing product by adopting an external standard method. The method is used for detecting the alkylphenol polyoxyethylene ether in the washing product, is good in separation effect of alkylphenol polyoxyethylene ether with different polymerization degrees, high in detection sensitivity, simple and convenient, and meets the demand of actual detection.
Description
Technical field
The present invention relates to a kind of detection method of articles for washing, relate in particular to the detection method of APES in a kind of articles for washing.
Background technology
Articles for washing is requisite household chemicals in people's daily life, at present, China has become the fastest country of urbanization process, and the process of Chinese Urbanization's has promoted people's living standard to improve greatly, has also promoted the fast development of prospect of Chinese washing products industry.According to latest data statistics, within 2012, prospect of Chinese washing products total production reaches 826.75 ten thousand tons.Meanwhile, the safety and effectiveness of articles for washing also becomes the Important Problems of relevant departments and consumers in general's concern.In articles for washing containing the multiple composition that health and ecologic environment is caused to potential hazard such as surfactant, musk xylene.In the 2003/53/EC of European Union instruction, the content of surfactant, musk xylene etc. in the product such as articles for washing, textile and cosmetics has all been done to clear and definite restriction.
Surfactant is a large class organic compound, has the multiple excellent functions such as dispersion, wetting, emulsification, solubilising, decontamination, foaming and froth breaking, widespread use in the industries such as articles for washing, herbicide, emulsifying agent, wetting agent, cosmetics, weaving.APES is the class non-ionics being made by alkyl phenol and reacting ethylene oxide, because it is wetting, infiltration, emulsification, dispersion, solubilising and washing etc. are functional, at present, in fields such as weaving, plastics, rubber, daily-use chemical industry, medicine, papermaking, electronics, be all widely used.In APES, NPE (NPE08) accounts for 80-85%, APES biodegradability is poor, catabolite in vivo has obvious eco-toxicity, can cause human internal environment and endocrine disturbance, thereby promote the growth of cancer cell, affect people's fecundity.European Union's 2003/53/EC instruction explicitly points out the use content of APES in chemicals and prepared product thereof lower than 0.1% (weight percent); in the < < environmental labelling product technical requirement one washing agent > > of China environmental protection cloth promulgated by the ministries or commissions of the Central Government, stipulate, in the washing agent such as fabric detergent, industrial detergent, must not use APES.
Analytical approach to APES etc. has UV, visible light spectrophotometric spectra method, infra-red sepectrometry, nuclear magnetic resonance method, liquid phase chromatography, MS, capillary electrophoresis etc., but the equal Shortcomings of said method and defect, can not meet the needs of actual detection.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of can to APES in articles for washing carry out fast detecting, method easy, detect method accurately, for the work such as the check of articles for washing and quality control provide technical support.
Technical scheme of the present invention is as follows:
A detection method for APES in articles for washing, comprises the following steps:
(1) accurately take APES standard items and be placed in right amount volumetric flask, add organic solvent constant volume, then with organic solvent diluting, prepare step by step the mark Huaihe River product solution of 3 kinds of desired concns;
(2) articles for washing that selection does not contain APES, as blank sample, adds organic solvent constant volume, then with organic solvent diluting, prepares step by step the reference substance solution of 3 kinds of desired concns;
(3) accurately take articles for washing sample and be placed in right amount color comparison tube, add organic solvent mixing constant volume, mix, ultrasonic extraction, finally adopts filtering with microporous membrane, gets filtrate for later use;
(4) to the articles for washing sample solution of preparation in abovementioned alkyl phenol polyethenoxy ether standard solution, reference substance solution and (2), adopt liquid chromatographic system to carry out qualitative and quantitative analysis; Method is carried out to linear relationship, the recovery and precision and investigate, finally to the content of APES in washing sample, adopt external standard method to measure.
In step (1), the compound method of APES standard solution is as follows: accurately take 5-10mg APES standard items, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is the APES standard solution of 0.05-0.1mg/mL; The APES standard solution that to get concentration that 10ml makes be 0.05-0.1mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.005-0.01mg/mL; ; The APES standard solution that to get the concentration that makes be 0.005-0.01mg/mL is again put in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.0005-0.001mg/mL;
In step (2), the compound method containing the reference substance solution of the articles for washing of APES is not as follows: accurately take 5-10mg containing the articles for washing of APES, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is 0.05-0.1mg/mL reference substance solution; Getting the concentration that 10ml makes is that 0.05-0.1mg/mL reference substance solution is placed in 100ml volumetric flask again, adds normal butane constant volume, mixes, and makes the reference substance solution that concentration is 0.005-0.01mg/mL; The reference substance solution that to get the concentration that makes be 0.005-0.01mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is 0.0005-0.001mg/mL reference substance solution;
In step (3), articles for washing sample solution compound method is as follows: accurately take 5-10mg articles for washing and be placed in 10ml color comparison tube, add mixed solvent to be settled to scale, mix, ultrasonic extraction 20-30min, cross after 0.45um miillpore filter, the filtrate of gained is articles for washing sample solution, and its concentration is 0.5-1.0mg/mL; Described mixed solvent is normal butane and the mixing of isopropyl alcohol, and the volume ratio of normal butane and isopropyl alcohol is 40:60; Described mixes as vortex mixes, and the instrument of employing is MS2 type vortex oscillation device; The instrument that ultrasonic extraction adopts is KQ-600B type ultrasonic cleaner.
In step (4), in liquid chromatographic system, normal butane, isopropyl alcohol are chromatographically pure, and it is pure that other reagent are analysis.
In step (4), in liquid chromatographic system, chromatographic condition is: chromatographic column: AgilentZORBAXNH2,5 μ m, mobile phase: A (80% normal butane-20% isopropyl alcohol, V/V), sample size is 10 μ L, flow velocity 1.5ml/min, 40 ℃ of column temperatures, detect wavelength 220-230nm.
The investigation concrete grammar of the linear relationship of described method, the recovery and precision is as follows:
(1) investigation of method linear relationship: by the accurate sample introduction of APES standard solution difference of the variable concentrations of preparation in step (1), the peak area sum (Y) of APES chromatographic peak of take is ordinate, sample size (X) is horizontal ordinate drawing standard curve, show that linear equation is Y=548.5X-4.25(r=0.9987).
(2) mensuration of the method recovery and precision: the APES standard solution of the variable concentrations of preparation in step (1) is joined respectively in the reference substance solution in step (2), the accurate sample introduction of difference, the recovery of investigation method and precision, the recovery of APES is 94.5-97.1%, and relative standard deviation is 2.5-4.8%.
Described external standard method concrete grammar is: under above-mentioned chromatographic condition, get the articles for washing sample solution and the accurate sample introduction of reference substance solution difference that prepare, record chromatogram and calculate by following formula: content (C
x)=C
r* (A
x/ A
r), (C
r: the concentration of reference substance; A
r: the peak area of reference substance or peak height; A
x: the peak area of testing sample or peak height).
Compared with prior art, beneficial effect has in the present invention:
1. APES is generally the polymkeric substance that a series of different polymerization degree APES monomeric compounds form, and because APES has the different degree of polymerization, its characteristic, toxicity and range of application all have larger difference.In reversed-phase liquid chromatography system, its hydrophobicity is depended in the separation of APES, the length that depends on alkyl carbon chain, the present invention adopts positive liquid chromatographic system, polyoxyethylene groups is identical and component that alkyl side chain is different can flow out jointly, therefore, the chromatographic peak of the APES of different polymerization degree overlaps, and separating effect is undesirable.In the present invention, adopt positive liquid chromatography cost of living system, ethoxy number is depended in the separation of APES, and ethoxy number can reach separated effect when different.Therefore, adopt the positive liquid chromatography in the present invention, to APES, can produce desirable separating effect, thereby the APES of different polymerization degree is carried out to qualitative and quantitative analysis.
2. the present invention adopts positive liquid chromatography to detect the APES method in articles for washing, have and detect rapidly, highly sensitive advantage, thereby the quality monitoring work that can carry out fast detecting and accurate quantitative analysis ，Wei relevant departments to the APES in actual life articles for washing provides practicable means.
In 3 the present invention, when articles for washing is dissolved, adopting volume ratio is the normal butane of 40:60 and the mixed solvent of isopropyl alcohol, and solute effect is better, and dissolution velocity is faster; Chromatographic column mobile phase adopts normal butane and the isopropyl alcohol that volume ratio is 80:20, has increased the partition factor of articles for washing, has improved separation efficiency.
Embodiment
The present invention, by the present invention of following specific embodiment more detailed description, can make those skilled in the art more fully understand the present invention, but not limit the present invention in any way.
Embodiment 1
(1) prepare the mark Huaihe River product solution of 3 kinds of desired concns: accurately take 5mg APES standard items, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is the APES standard solution of 0.05mg/mL; The APES standard solution that to get concentration that 10ml makes be 0.05mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.005mg/mL; ; The APES standard solution that to get the concentration that makes be 0.005mg/mL is again put in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.0005mg/mL;
(2) prepare the reference substance solution of 3 kinds of desired concns: accurately take 5mg not containing the articles for washing (liquid detergent) of APES, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is 0.05mg/mL reference substance solution; Getting the concentration that 10ml makes is that 0.05mg/mL reference substance solution is placed in 100ml volumetric flask again, adds normal butane constant volume, mixes, and makes the reference substance solution that concentration is 0.005mg/mL; The reference substance solution that to get the concentration that makes be 0.005mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is 0.0005mg/mL reference substance solution;
(3) sample solution of preparation articles for washing: accurately take 5mg articles for washing (liquid detergent) and be placed in 10ml color comparison tube, add normal butane that volume ratio is 40:60 and the mixed solvent of isopropyl alcohol to be settled to scale, adopting MS2 type vortex oscillation device contrast colour tube to carry out vortex mixes, the instrument adopting is the ultrasonic extraction of KQ-600B type ultrasonic cleaner 20min, cross after 0.45 μ m miillpore filter, make the articles for washing sample solution of 0.5mg/mL;
(4) to the articles for washing sample solution of preparation in abovementioned alkyl phenol polyethenoxy ether standard solution, reference substance solution and (2), adopt liquid chromatographic system to carry out qualitative and quantitative analysis; In liquid chromatographic system, normal butane, isopropyl alcohol are chromatographically pure, and it is pure that other reagent are analysis; Chromatographic condition: chromatographic column: AgilentZORBAX NH2,5 μ m, mobile phase: A (80% normal butane-20% isopropyl alcohol, V/V), sample size is 10 μ L, flow velocity 1.5ml/min, 40 ℃ of column temperatures, detect wavelength 220nm.
(5) method is carried out to the investigation of linear relationship, the recovery and precision:
The investigation of method linear relationship: by the accurate sample introduction of APES standard solution difference of the variable concentrations of preparation, the peak area sum (Y) of APES chromatographic peak of take is ordinate, sample size (X) is horizontal ordinate drawing standard curve, show that linear equation is Y=548.5X-4.25(r=0.9987);
The mensuration of the method recovery and precision: the APES standard solution of variable concentrations is joined respectively in the reference substance solution of variable concentrations, the accurate sample introduction of difference, the recovery of investigation method and precision, the recovery of APES is 94.5%, and relative standard deviation is 2.5%.
(6) to the APES in articles for washing (liquid detergent), adopt external standard method to carry out assay: under above-mentioned chromatographic condition, get the articles for washing sample solution and the accurate sample introduction of reference substance solution difference that prepare, record chromatogram and calculate by following formula: content (C
x)=C
r* (A
x/ A
r), (C
r: the concentration of reference substance; A
r: the peak area of reference substance or peak height; A
x: the peak area of testing sample or peak height).
In measuring and calculating articles for washing (liquid detergent), APES content is 0.15%, does not meet the standard of China's current edition to APES content in articles for washing.
Embodiment 2:
(1) prepare the mark Huaihe River product solution of 3 kinds of desired concns: accurately take 10mg APES standard items, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is the APES standard solution of 0.1mg/mL; The APES standard solution that to get concentration that 10ml makes be 0.1mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.01mg/mL; ; The APES standard solution that to get the concentration that makes be 0.01mg/mL is again put in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.001mg/mL;
(2) prepare the reference substance solution of 3 kinds of desired concns: accurately take 10mg not containing the articles for washing (liquid detergent) of APES, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is 0.1mg/mL reference substance solution; Getting the concentration that 10ml makes is that 0.1mg/mL reference substance solution is placed in 100ml volumetric flask again, adds normal butane constant volume, mixes, and makes the reference substance solution that concentration is 0.01mg/mL; The reference substance solution that to get the concentration that makes be 0.01mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is 0.001mg/mL reference substance solution;
(3) sample solution of preparation articles for washing: accurately take 10mg articles for washing (liquid detergent) and be placed in 10ml color comparison tube, add normal butane that volume ratio is 40:60 and the mixed solvent of isopropyl alkane to be settled to scale, adopting MS2 type vortex oscillation device contrast colour tube to carry out vortex mixes, the instrument adopting is the ultrasonic extraction of KQ-600B type ultrasonic cleaner 20min, cross after 0.45um miillpore filter, make the articles for washing sample solution of 1mg/mL;
(4) to the articles for washing sample solution of preparation in abovementioned alkyl phenol polyethenoxy ether standard solution, reference substance solution and (2), adopt liquid chromatographic system to carry out qualitative and quantitative analysis; In liquid chromatographic system, normal butane, isopropyl alcohol are chromatographically pure, and it is pure that other reagent are analysis; Chromatographic condition: chromatographic column: AgilentZORBAX NH2,5 μ m, mobile phase: A (80% normal butane-20% isopropyl alcohol, V/V), sample size is 10 μ L, flow velocity 1.5ml/min, 40 ℃ of column temperatures, detect wavelength 230nm.
(5) method is carried out to the investigation of linear relationship, the recovery and precision:
The investigation of method linear relationship: by the accurate sample introduction of APES standard solution difference of the variable concentrations of preparation, the peak area sum (Y) of APES chromatographic peak of take is ordinate, sample size (X) is horizontal ordinate drawing standard curve, show that linear equation is Y=578.5X-4.05(r=0.9989);
The mensuration of the method recovery and precision: the APES standard solution of variable concentrations is joined respectively in the reference substance solution of variable concentrations, the accurate sample introduction of difference, the recovery of investigation method and precision, the recovery of APES is 97.1%, and relative standard deviation is 4.8%.
(6) to the APES in articles for washing (liquid detergent), adopt external standard method to carry out assay: under above-mentioned chromatographic condition, get the articles for washing sample solution and the accurate sample introduction of reference substance solution difference that prepare, record chromatogram and calculate by following formula: content (C
x)=C
r* (A
x/ A
r), (C
r: the concentration of reference substance; A
r: the peak area of reference substance or peak height; A
x: the peak area of testing sample or peak height).
In measuring and calculating articles for washing (washing powder), APES content is 0.13%, does not meet the standard of China's current edition to APES content in articles for washing.
Embodiment 3:
(1) prepare the mark Huaihe River product solution of 3 kinds of desired concns: accurately take 8mg APES standard items, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is the APES standard solution of 0.08mg/mL; The APES standard solution that to get concentration that 10ml makes be 0.08mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.008mg/mL; ; The APES standard solution that to get the concentration that makes be 0.008mg/mL is again put in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.0008mg/mL;
(2) prepare the reference substance solution of 3 kinds of desired concns: accurately take 8mg not containing the articles for washing (liquid detergent) of APES, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is 0.08mg/mL reference substance solution; Getting the concentration that 10ml makes is that 0.08mg/mL reference substance solution is placed in 100ml volumetric flask again, adds normal butane constant volume, mixes, and makes the reference substance solution that concentration is 0.008mg/mL; The reference substance solution that to get the concentration that makes be 0.008mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is 0.0008mg/mL reference substance solution;
(3) sample solution of preparation articles for washing: accurately take 8mg articles for washing (hand cleanser) and be placed in 10ml color comparison tube, add normal butane that volume ratio is 40:60 and the mixed solvent of isopropyl alkane to be settled to scale, adopting MS2 type vortex oscillation device contrast colour tube to carry out vortex mixes, the instrument adopting is the ultrasonic extraction of KQ-600B type ultrasonic cleaner 20min, cross after 0.45um miillpore filter, make the articles for washing sample solution of 1mg/mL;
(4) to the articles for washing sample solution of preparation in abovementioned alkyl phenol polyethenoxy ether standard solution, reference substance solution and (2), adopt liquid chromatographic system to carry out qualitative and quantitative analysis; In liquid chromatographic system, normal butane, isopropyl alcohol are chromatographically pure, and it is pure that other reagent are analysis; Chromatographic condition: chromatographic column: AgilentZORBAX NH2,5 μ m, mobile phase: A (80% normal butane-20% isopropyl alcohol, V/V), sample size is 10 μ L, flow velocity 1.5ml/min, 40 ℃ of column temperatures, detect wavelength 230nm.
(5) method is carried out to the investigation of linear relationship, the recovery and precision:
The investigation of method linear relationship: by the accurate sample introduction of APES standard solution difference of the variable concentrations of preparation, the peak area sum (Y) of APES chromatographic peak of take is ordinate, sample size (X) is horizontal ordinate drawing standard curve, show that linear equation is Y=558.5X-4.12(r=0.9991);
The mensuration of the method recovery and precision: the APES standard solution of variable concentrations is joined respectively in the reference substance solution of variable concentrations, the accurate sample introduction of difference, the recovery of investigation method and precision, the recovery of APES is 95.8%, and relative standard deviation is 3.4%.
(6) to the APES in articles for washing (hand cleanser), adopt external standard method to carry out assay: under above-mentioned chromatographic condition, get the articles for washing sample solution and the accurate sample introduction of reference substance solution difference that prepare, record chromatogram and calculate by following formula: content (C
x)=C
r* (A
x/ A
r), (C
r: the concentration of reference substance; A
r: the peak area of reference substance or peak height; A
x:the peak area of testing sample or peak height).
In measuring and calculating articles for washing (hand cleanser), APES content is 0.05%, meets the standard of China's current edition to APES content in articles for washing.
The above embodiment is preferred embodiments of the present invention, is not to limit the scope of the present invention, and the equivalence of doing according to structure, feature and principle described in the present patent application the scope of the claims therefore all changes or modifies, and all should comprise in patent claim of the present invention.
Claims (10)
1. a detection method for APES in articles for washing, is characterized in that, comprises the following steps:
(1) take APES standard items and be placed in volumetric flask, add organic solvent constant volume, then with organic solvent diluting, prepare step by step the mark Huaihe River product solution of 3 kinds of desired concns;
(2) articles for washing that selection does not contain APES, as blank sample, adds organic solvent constant volume, then with organic solvent diluting, prepares step by step the reference substance solution of 3 kinds of desired concns;
(3) take articles for washing sample and be placed in color comparison tube, add organic solvent mixing constant volume, mix, ultrasonic extraction, finally adopts filtering with microporous membrane, gets filtrate for later use;
(4) to the articles for washing sample solution making in the reference substance solution making in the APES standard solution making in step (1), step (2) and step (3), adopt liquid chromatographic system to carry out qualitative and quantitative analysis; Method is carried out to linear relationship, the recovery and precision and investigate, finally to the content of APES in washing sample, adopt external standard method to measure.
2. the detection method of APES in a kind of articles for washing according to claim 1, it is characterized in that, in step (1), the compound method of APES standard solution is as follows: accurately take 5-10mg APES standard items, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is the APES standard solution of 0.05-0.1mg/mL; The APES standard solution that to get concentration that 10ml makes be 0.05-0.1mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.005-0.01mg/mL; ; The APES standard solution that to get the concentration that makes be 0.005-0.01mg/mL is again put in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is the APES standard solution of 0.0005-0.001mg/mL.
3. the detection method of APES in a kind of articles for washing according to claim 1, it is characterized in that, in step (2), the compound method containing the reference substance solution of the articles for washing of APES is not as follows: accurately take 5-10mg containing the articles for washing of APES, be placed in 100ml volumetric flask, add normal butane constant volume, mix, making concentration is 0.05-0.1mg/mL reference substance solution; Getting the concentration that 10ml makes is that 0.05-0.1mg/mL reference substance solution is placed in 100ml volumetric flask again, adds normal butane constant volume, mixes, and makes the reference substance solution that concentration is 0.005-0.01mg/mL; The reference substance solution that to get the concentration that makes be 0.005-0.01mg/mL is again placed in 100ml volumetric flask, adds normal butane constant volume, mixes, and making concentration is 0.0005-0.001mg/mL reference substance solution.
4. the detection method of APES in a kind of articles for washing according to claim 1, it is characterized in that, in step (3), articles for washing sample solution compound method is as follows: accurately take 5-10mg articles for washing and be placed in 10ml color comparison tube, add mixed solvent to be settled to scale, mix, ultrasonic extraction 20-30min, crosses after 0.45um miillpore filter, the filtrate of gained is articles for washing sample solution, and its concentration is 0.5-1.0mg/mL.
5. the detection method of APES in a kind of articles for washing according to claim 4, is characterized in that, described mixed solvent is normal butane and the mixing of isopropyl alcohol, and the volume ratio of normal butane and isopropyl alkane is 40:60.
6. the detection method of APES in a kind of articles for washing according to claim 4, is characterized in that, described mixes as vortex mixes, and the instrument of employing is MS2 type vortex oscillation device; The instrument that ultrasonic extraction adopts is KQ-600B type ultrasonic cleaner.
7. the detection method of APES in a kind of articles for washing according to claim 1, is characterized in that, in step (4), in liquid chromatographic system, normal butane, isopropyl alcohol are chromatographically pure, and it is pure that other reagent are analysis.
8. the detection method of APES in a kind of articles for washing according to claim 1, it is characterized in that, in step (4), in liquid chromatographic system, chromatographic condition is: chromatographic column: AgilentZORBAXNH2,5 μ m, and mobile phase: A (80% normal butane-20% isopropyl alcohol, V/V), sample size is 10 μ L, flow velocity 1.5ml/min, 40 ℃ of column temperatures, detect wavelength 220-230nm.
9. the detection method of APES in a kind of articles for washing according to claim 1, is characterized in that, the investigation concrete grammar of the linear relationship of described method, the recovery and precision is as follows:
(1) investigation of method linear relationship: by the accurate sample introduction of APES standard solution difference of the variable concentrations of preparation in step (1), the peak area sum (Y) of APES chromatographic peak of take is ordinate, sample size (X) is horizontal ordinate drawing standard curve, draws linear equation;
(2) mensuration of the method recovery and precision: the APES standard solution of the variable concentrations of preparation in step (1) is joined respectively in the reference substance solution in step (2), the accurate sample introduction of difference, the recovery of investigation method and precision, the recovery of APES is 94.5-97.1%, and relative standard deviation is 2.5-4.8%.
10. the detection method of APES in a kind of articles for washing according to claim 1, it is characterized in that, described external standard method concrete grammar is: under above-mentioned chromatographic condition, get the articles for washing sample solution and the accurate sample introduction of reference substance solution difference that prepare, record chromatogram and calculate by following formula: content (C
x)=C
r* (A
x/ A
r), (C
r: the concentration of reference substance; A
r: the peak area of reference substance or peak height; A
x: the peak area of testing sample or peak height).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699571A (en) * | 2016-03-18 | 2016-06-22 | 中华人民共和国鄞州出入境检验检疫局 | Method for determining short-chain p-tert-octyl phenol ethoxylate in textiles |
| CN106053588A (en) * | 2016-06-02 | 2016-10-26 | 中国检验检疫科学研究院 | Rapid detection method of alkylphenol ethoxylate on basis of ion mobility spectrometry |
| CN110954639A (en) * | 2019-12-16 | 2020-04-03 | 中国计量大学 | Analysis method of styrylphenol polyoxyethylene ether surfactant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539368A (en) * | 2012-01-16 | 2012-07-04 | 浙江理工大学 | Spectrum detection method for alkylphenol compounds in textile auxiliaries |
| CN103018385A (en) * | 2012-11-21 | 2013-04-03 | 国家皮革质量监督检验中心（浙江） | Gas chromatography-mass spectrometry detection method for nonylphenol polyoxyethylene ether in toilet cleaner |
| CN103175933A (en) * | 2013-02-20 | 2013-06-26 | 广州市质量监督检测研究院 | Method for quantitatively detecting alkylphenol polyoxyethylene in daily chemical products |
-
2013
- 2013-11-28 CN CN201310614750.3A patent/CN103630625A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539368A (en) * | 2012-01-16 | 2012-07-04 | 浙江理工大学 | Spectrum detection method for alkylphenol compounds in textile auxiliaries |
| CN103018385A (en) * | 2012-11-21 | 2013-04-03 | 国家皮革质量监督检验中心（浙江） | Gas chromatography-mass spectrometry detection method for nonylphenol polyoxyethylene ether in toilet cleaner |
| CN103175933A (en) * | 2013-02-20 | 2013-06-26 | 广州市质量监督检测研究院 | Method for quantitatively detecting alkylphenol polyoxyethylene in daily chemical products |
Non-Patent Citations (5)
| Title |
|---|
| 乔玉霜: "壬基酚和短链壬基酚聚氧乙烯醚同时分析的方法建立", 《中国环境监测》 * |
| 刘欣 等: "正相高效液相色谱法分离检测壬基酚和短链壬基酚聚氧乙烯醚", 《分析化学》 * |
| 吕爱丽 等: "纺织品中壬基酚聚氧乙烯醚检测方法的研究", 《毛纺科技》 * |
| 马强 等: "正相液相色谱法测定洗涤用品中的烷基酚聚氧乙烯醚", 《分析试验室》 * |
| 马强 等: "烷基酚聚氧乙烯醚在不同液相色谱分离模式中的分离研究", 《分析测试学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699571A (en) * | 2016-03-18 | 2016-06-22 | 中华人民共和国鄞州出入境检验检疫局 | Method for determining short-chain p-tert-octyl phenol ethoxylate in textiles |
| CN106053588A (en) * | 2016-06-02 | 2016-10-26 | 中国检验检疫科学研究院 | Rapid detection method of alkylphenol ethoxylate on basis of ion mobility spectrometry |
| CN106053588B (en) * | 2016-06-02 | 2018-08-17 | 中国检验检疫科学研究院 | A kind of rapid detection method of the alkyl phenol polyoxyethylene ether based on ion mobility spectrometry |
| CN110954639A (en) * | 2019-12-16 | 2020-04-03 | 中国计量大学 | Analysis method of styrylphenol polyoxyethylene ether surfactant |
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