CN102338790B - Method for measuring fatty acid soap in amino acid surface active agent - Google Patents
Method for measuring fatty acid soap in amino acid surface active agent Download PDFInfo
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Abstract
The invention relates to a method for measuring the fatty acid soap in an amino acid surface active agent, which comprises the following steps: acidizing the surface active agent; extracting converted organic acid by using an organic solvent; then carrying out esterification; and finally, measuring the content of ester by using a gas chromatograph through an internal standard method to obtain the content of the fatty acid soap. The method is simple, convenient and rapid and is suitable for trace analysis in chemical production.
Description
Technical field
The present invention relates to a kind of assay method of fatty acid soap in amino acid surface active agent content.By method of the present invention, can analyze fast the content of fatty acid soaps in the intermediate of amino acid surfactant and even end product, be applicable to middle control analysis, trace analysis and the product analysis etc. of Chemical Manufacture.
Background technology
In recent years, for the needs to environmental protection and biological safety, exploitation and environment for use close friend's surfactant is subject to the attention of countries in the world day by day, and amino acid type surfactant is wherein a kind of, well received.It has good wetting state, foamability, antibiotic property etc., almost non-toxic harmless, to skin gentleness, its catabolite is amino acid and fatty acid, therefore on almost no impact of environment, but also have advantages of with other various surfactant compatibility well, can be widely used in personal cleanliness's articles for use such as cosmetics (mildy wash, shower cream, shampoo, facial mask etc.), washing agent, medical and health and personal care articles.
Because amino acid surfactant often reacts synthetic by Schotten-Baumann, therefore in the reaction of amino acid surfactant, can contain accessory substance fatty acid soaps, along with the number of fatty acid soaps content, the scourability, wettability and the foaming capacity that have affected this surfactant all can decline thereupon, so it is most important to guaranteeing the quality of surfactant to control the content of accessory substance fatty acid soaps.The content of analyzing fatty acid soaps in amino acid surfactant is a difficult problem.The analytical approach that some offshore company is used is to utilize zeyssatite chromatography method, but the zeyssatite that uses internal reagent company to buy carries out chromatography, and analysis result is dissatisfied.Method operation is more loaded down with trivial details, consuming time also long, and reappearance is good not, as the rather inconvenience of trace analysis of daily production.
For the problems referred to above, the inventor provides the assay method that a kind of relative cost is lower, easy and simple to handle.The method can faster analyze the content of fatty acid soaps in the intermediate of surfactant and end product by acidifying, esterification and gas chromatographic analysis, because this method is consuming time shorter, operate simpler, preci-sion and accuracy is all more satisfied, is therefore applicable to the middle of amino acid surfactant and controls and check analysis.
Summary of the invention
The object of the invention is to provide a kind of assay method of fatty acid soap in amino acid surface active agent content.
Method of the present invention is first by the mineral acid acidifying of this surfactant, is preferably less than 1 to pH, and the organic acid then generating with organic solvent extraction, collects extract, then except organic solvent, as with hot bath or rotary evaporation in vacuo evaporate to dryness sample; Add the alcoholic solution of catalyzer to reflux in above-mentioned sample and carry out esterification, the product of esterification is used solvent extraction again; Collect extract, add a certain amount of fatty alcohol internal standard compound, use methyl laurate as standard specimen simultaneously, configure respectively standard solution and test solution, standard solution and test solution are measured by vapor-phase chromatography, can determine the content of ester in product, thereby extrapolate the content of fatty acid soaps.
The organic solvent of the extraction adopting is the non-polar solvents such as benzene, dimethylbenzene, ether and sherwood oil.
Described esterification process is preferably esterification, esterification 0.5---5 hour.
Described fatty alcohol Selection of internal standard hexadecanol or 18 alcohol.
The detecting device of described vapor-phase chromatography is selected hydrogen flame detector FID, and chromatographic column is selected non-polar column, adopts temperature programme, internal standard method, and last computing formula is:
In formula:
SM
1---the peak area of internal standard compound fatty alcohol in sample
WA
1---the example weight after caproic acid constant weight
SA
1---the peak area of methyl laurate in sample after esterification
WA
2---the weight of methyl laurate in standard specimen
SA
2---the peak area of methyl laurate in standard specimen
SM
2---the peak area of internal standard compound fatty alcohol in standard specimen
The present invention uses zeyssatite chromatography method cost lower, easy and simple to handle relatively, and the reagent of use is laboratory common agents, and pretreated process is not loaded down with trivial details yet.The method is exactly to analyze these by acidifying, esterification, gas chromatograph to process easily the content that just can analyze fast fatty acid soaps in the intermediate of surfactant and even end product, because this method is consuming time short, simple to operate, be applicable to middle control and the trace analysis etc. of the daily production in chemical plant.
Embodiment
Contribute to understand the present invention by instantiation below, but do not limit the scope of application of the present invention.
Embodiment 1
Acidifying: get 30g sample, be placed in separating funnel, adding distil water and the concentrated sulphuric acid, recommend to PH≤1.Add 75mL xylene extraction, after layering, emit lower aqueous layer.Add again 50mL distilled water, after jolting washing, emit water layer.With qualitative filter paper filter xylene solution to 250mL 24
#in ground round-bottomed bottle.Rotary evaporation in vacuo it, vacuum is drained sample, in clean to of sample wide-necked bottle.
Esterification: take the synthetic product of 2.5g caproic acid, constant weight in round-bottomed flask, add the methanol solution 80mL of p-methyl benzenesulfonic acid, esterification 5h refluxes in water-bath, after esterification, be poured in separating funnel, with 3 washing esterification flasks of 100mL distillation moisture, merge 3 cleansing solutions in separating funnel, divide 3 extractions with 20mL sherwood oil, the 1st 10mL, use respectively 10.0mL petroleum ether extraction the 2nd time and the 3rd time, petroleum ether layer is collected in 50mL volumetric flask, adds mark liquid in 10mL, finally be diluted to scale with sherwood oil, shake up as sample for subsequent use.
Gas chromatography analysis method
The preparation of interior mark liquid: take 2.0g 18 alcohol in 100mL volumetric flask, by xylene soluble and be diluted to scale, shake up for subsequent use.
The preparation of standard model: take 0.2g methyl laurate in 50mL volumetric flask, add 10mL sherwood oil molten even, accurately pipette in 10mL and mark liquid in volumetric flask with transfer pipet, be finally diluted to scale with sherwood oil, shake up for subsequent use.
Analytical conditions for gas chromatography (internal standard method):
Detecting device: flame ionization ditector (FID)
Chromatographic column: non-polar column HP-1 15m × 0.53mm × 1.5 μ m or suitable
Temperature of vaporization chamber: 200 DEG C of detector temperatures: 200 DEG C
Column temperature: 100-200 DEG C of temperature programme programming rate: 10 DEG C/min
Gas flow rate: nitrogen 60mL/min, hydrogen 50mL/min, air 0.9L/min
Sample size: 0.2 μ L
Result is calculated:
Record with the fatty acid soaps content data in a collection of sodium lauroyl sarcosine following (Precision Experiment data)
Embodiment 2
Acidifying: get 30g sample, be placed in separating funnel, adding distil water and concentrated hydrochloric acid, to PH≤1.Add 75mL extracted with diethyl ether, after layering, emit lower aqueous layer.Add again 50mL distilled water, after jolting washing, emit water layer.With qualitative filter paper filter diethyl ether solution to 250mL 24
#in ground round-bottomed bottle.Rotary evaporation in vacuo it, vacuum is drained sample, in clean to of sample wide-necked bottle.
Esterification: take the synthetic product of 2g caproic acid, constant weight in round-bottomed flask, add the methanol solution 80mL of p-methyl benzenesulfonic acid, esterification 2h refluxes in water-bath, after esterification, be poured in separating funnel, with 3 washing esterification flasks of 100mL distillation moisture, merge 3 cleansing solutions in separating funnel, divide 3 extractions with 20mL sherwood oil, the 1st 10mL, use respectively 10.0mL petroleum ether extraction the 2nd time and the 3rd time, petroleum ether layer is collected in 50mL volumetric flask, adds mark liquid in 10mL, finally be diluted to scale with sherwood oil, shake up as sample for subsequent use.
Gas chromatography analysis method
The preparation of interior mark liquid: take 2.0g hexadecanol in 100mL volumetric flask, by xylene soluble and be diluted to scale, shake up for subsequent use.
The preparation of standard model: take 0.2g methyl laurate in 50mL volumetric flask, add 10mL sherwood oil molten even, accurately pipette in 10mL and mark liquid in volumetric flask with transfer pipet, be finally diluted to scale with sherwood oil, shake up for subsequent use.
Analytical conditions for gas chromatography (internal standard method):
Detecting device: flame ionization ditector (FID)
Chromatographic column: non-polar column HP-1 15m × 0.53mm × 1.5 μ m or suitable
Temperature of vaporization chamber: 300 DEG C of detector temperatures: 300 DEG C
Column temperature: 100-260 DEG C of temperature programme programming rate: 8 DEG C/min
Gas flow rate: nitrogen 60mL/min, hydrogen 50mL/min, air 0.9L/min
Sample size: 0.2 μ L
The inventive method has been carried out to precision and measured and accuracy determination, method is as follows:
Precision is measured: selected with a collection of sodium lauroyl sarcosine product, under identical experiment condition, (reagent, instrument, operating personnel etc.), to six groups of data of its replicate determination, draw the lauric acid soap content of this product and calculate precision.
Accuracy determination: take 0.1000g (being accurate to 0.0002) lauric acid (content: 98.0%) in 100mL volumetric flask, molten even and be diluted to scale with methyl alcohol, shake up.Accurately pipette respectively 2ml with transfer pipet, 4ml, 6ml, 8ml to above-mentioned sample to pretreated the said goods of known lauric acid soap content in, again measure lauric acid soap content by gas chromatograph internal standard method.
Result is calculated:
Record with the fatty acid soaps content data in a collection of sodium lauroyl sarcosine following (Precision Experiment data)
Accuracy test data
Claims (7)
1. an assay method for fatty acid soap in amino acid surface active agent content, is characterized in that the mineral acid acidifying of this surfactant, pH≤1 after acidifying, the organic acid that organic solvent extraction has transformed; Extract carries out esterification except after organic solvent, and esterification products is used organic solvent extraction again, and extract as standard specimen, adds internal standard compound fatty alcohol with methyl laurate, with the content of ester in gas chromatograph for determination product;
The detecting device of described gas chromatograph is selected hydrogen flame detector, and chromatographic column is selected non-polar column, use be internal standard method; Procedure for selection heats up, and temperature of vaporization chamber and detector temperature are all greater than 200 DEG C; 100-300 DEG C of temperature programme, programming rate is 5～10 DEG C/min;
Described internal standard compound is that fatty alcohol is hexadecanol or 18 alcohol; Obtain the content of fatty acid soaps according to following formula:
In formula:
SM
1---the peak area of internal standard compound fatty alcohol in sample
WA
1---the example weight after acidifying constant weight
SA
1---the peak area of methyl laurate in sample after esterification
WA
2---the weight of methyl laurate in standard specimen
SA
2---the peak area of methyl laurate in standard specimen
SM
2---the peak area of internal standard compound fatty alcohol in standard specimen.
2. the method for claim 1, is characterized in that described mineral acid is hydrochloric acid, sulfuric acid, phosphoric acid or nitric acid.
3. the method for claim 1, is characterized in that the organic solvent using after described acidifying and esterification is benzene, dimethylbenzene, ether or sherwood oil.
4. the method for claim 1, is characterized in that described esterification is to add alcoholic solution and catalyzer after extract removes organic solvent, refluxes and within 0.5～5 hour, carries out esterification.
5. method as claimed in claim 4, is characterized in that described alcohol is methyl alcohol.
6. method as claimed in claim 4, is characterized in that described catalyzer is sulfuric acid, phosphoric acid or p-toluenesulfonic acid.
7. the method for claim 1, is characterized in that the mineral acid acidifying of this surfactant, pH≤1 after acidifying, the organic acid that organic solvent extraction has transformed; Extract carries out esterification except after organic solvent,
Esterification products is used organic solvent extraction again, and extract as standard specimen, adds internal standard compound fatty alcohol with methyl laurate, with the content of ester in gas chromatograph for determination product;
Analytical conditions for gas chromatography: detecting device: flame ionization ditector FID; Chromatographic column: non-polar column HP-115m × 0.53mm × 1.5 μ m; Temperature of vaporization chamber: 200 DEG C; Detector temperature: 200 DEG C; Column temperature: 100-200 DEG C temperature programme; Programming rate: 10 DEG C/min; Gas flow rate: nitrogen 60mL/min; Hydrogen 50mL/min; Air 0.9L/min; Sample size: 0.2 μ L; Or detecting device: flame ionization ditector FID; Chromatographic column: non-polar column HP-115m × 0.53mm × 1.5 μ m; Temperature of vaporization chamber: 300 DEG C; Detector temperature: 300 DEG C; Column temperature: 100-260 DEG C temperature programme; Programming rate: 8 DEG C/min; Gas flow rate: nitrogen 60mL/min; Hydrogen 50mL/min; Air 0.9L/min; Sample size: 0.2 μ L;
Described internal standard compound is that fatty alcohol is hexadecanol or 18 alcohol; Obtain the content of fatty acid soaps according to following formula:
In formula:
SM
1---the peak area of internal standard compound fatty alcohol in sample
WA
1---the example weight after acidifying constant weight
SA
1---the peak area of methyl laurate in sample after esterification
WA
2---the weight of methyl laurate in standard specimen
SA
2---the peak area of methyl laurate in standard specimen
SM
2---the peak area of internal standard compound fatty alcohol in standard specimen.
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| CN105675749B (en) * | 2016-01-15 | 2017-07-18 | 广州天赐高新材料股份有限公司 | The analysis method of cocoyl amino acid surfactant carbochain composition |
| CN106442829B (en) * | 2016-12-13 | 2018-01-02 | 广州天赐高新材料股份有限公司 | It is a kind of while detect the method for aliphatic acid and active matter content in fatty acyl neutral amino acid surfactant |
| CN112268964A (en) * | 2020-09-28 | 2021-01-26 | 江苏集萃新型药物制剂技术研究所有限公司 | Method for measuring content of hexadecanol and octadecanol in medicinal preparation |
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