CN101520442B - High efficiency liquid chromatograph analysis method for sodium isethionate - Google Patents
High efficiency liquid chromatograph analysis method for sodium isethionate Download PDFInfo
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- CN101520442B CN101520442B CN2009100262569A CN200910026256A CN101520442B CN 101520442 B CN101520442 B CN 101520442B CN 2009100262569 A CN2009100262569 A CN 2009100262569A CN 200910026256 A CN200910026256 A CN 200910026256A CN 101520442 B CN101520442 B CN 101520442B
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Abstract
The invention provides a high efficiency liquid chromatograph analysis method for sodium isethionate, which relates to an HPLC-ELSD analysis method for analyzing the content of impurities of fatty acyl sulfonate. The invention makes use of the high efficiency liquid chromatography analysis method and an evaporative light-scattering detector to measure the content of the sodium isethionate with a standard curve method; and a sample is dissolved with methanol, methanol-water is used as a mobile phase, a stainless steel column using Lichrospher-C18 as a filler and the evaporative light-scattering detector are used, the recovery rate is between 95.2 and 98.3 percent, the detection limit is 0.02 mu g/mL, and the precision RSD is less than 3.00 percent. The method uses popularized instruments and has simple steps, and the measuring result is verified by the conventional ion chromatography method, is correct and reliable, and has high sensitivity and good reproducibility. The invention discloses a sensitive, rapid and simple high efficiency liquid chromatograph method for detecting the content of the sodium isethionate (SI), which controls the SI content in the formulation of a solid synthetic detergent soap to further play an important role in quality control of products.
Description
Technical field
A kind of HPLC analytical method of sodium isethionate the present invention relates to high performance liquid chromatography evaporative light-scattering detecting device (HPLC-ELSD) analytic approach.Specifically, relate to and use the HPLC-ELSD analytic approach, analyze the content of fatty acyl group sulphonate impurity.
Background technology
Yi Jiebang A (Igepon A) is the less relatively anionic surfactant of pungency, and is insensitive to hard water, and good foaming properties and detergency are arranged, good to the skin compatibility of human body, is widely used in cosmetics and the detergent compositions.The raw materials for production of Igepon A mainly are fatty acid (great majority are cocinic acids) and sodium isethionate (SI).When producing Igepon A, have neither part nor lot in the product esterification the SI residual volume confirm extremely important to the arrangement stage of soapmaking process, if in the soapmaking process in the soap amount of SI can be controlled in a certain scope, can significantly improve the hardness and the processing characteristics of soap.The minority isethionate can be used as the hardening agent of block perfumed soap, and the raising of hardness is played a role to the shaping ability that increases soap.In the solid soap prescription; SI content also produces very large influence to the usability of soap; Content like SI in the soap has surpassed certain limit; Can produce certain pungency to skin,, measure necessary the content of residual SI among the Igepon A so SI content is an important index to production quality control.
But about the assay of residual SI, never the article report does not more have the relevant criterion issue in the Igepon A quality index.Chromatography of ions is that present p-sulfonic acid salt content is analyzed mature methods, but the use of chromatography of ions is universal far away from high performance liquid chromatography.HPLC-ELSD provided by the invention analyzes the method for SI, is a kind of method that is easy to popularize, and the production run that can be used for Igepon A and soap detects, in the product quality detection.
Summary of the invention
The efficient liquid-phase chromatography method that the purpose of this invention is to provide a kind of sensitivity, quick, easy detection SI content.
Technical scheme of the present invention: the HPLC analytical method of a kind of sodium isethionate SI, adopt high performance liquid chromatography, cooperate EISD, measure the isethionic acid sodium content with calibration curve method.Because of Igepon A and SI are sulphonate, uv absorption extremely a little less than, can't select UV-detector as checkout equipment.Though differential refraction detector is universal detecting device,, can not satisfy the requirement that low concentration is analyzed because its sensitivity is too low, and is subject to the influence of external environment fluctuation.When selecting the high-efficient liquid phase chromatogram technique analysis alkyl sulfonate for use, except that the separation condition of seeking, also to select suitable detection system.So this method adopts the higher EISD of sensitivity to measure.
The high performance liquid chromatography operating conditions is:
The stainless steel column of chromatographic column: 250mm * 4.6mm (id), Lichrospher-5 μ m-C
18Filler;
Moving phase is formed volume ratio: methyl alcohol: ultrapure water=100～50: 0～50; Recommending volume ratio is 100～80: 0～20;
Flow velocity: 0.2～1.2mL/min; The recommendation flow velocity is 0.3～0.8mL/min;
Column temperature: 10～60 ℃; Recommend column temperature: 25～50 ℃;
Detecting device: EISD;
Jet chamber's rank 50%～80% of detecting device; Recommending jet chamber's rank of detecting device is 60%;
40～60 ℃ of drift tube temperatures; Recommending drift tube temperature is 40～50 ℃;
Nitrogen pressure 15～40psi; The recommendation nitrogen pressure is 20psi.
Reference material: adopt the SI powder of >=99% purity or the SI WS of massfraction 48%.Recommend to adopt the SI powder of >=99% purity.
The sampling volume of high performance liquid chromatography operation adopts conventional parameter, and recommending sample size is 20 μ L.
Recommend the used ultrapure water of described moving phase, through boiling, to remove O
2And CO
2Deng dissolved gas; Described moving phase is used ultrasonic degas before use.
Beneficial effect of the present invention: the present invention adopts the HPLC-ELSD analytic approach, analyzes fatty acyl group sulphonate impurity content, and the result of mensuration obtains the checking of traditional chromatography of ions, and is correct reliable.That this method has is highly sensitive, detectability is low, precision good, speed is fast, the efficient advantages of higher; Requiring operating personnel to learn molten (notes) sample just can accurately analyze; Be applicable to factory's On-line Control analysis and batch samples analysis; Further perfect along with this method will provide certain reference value for the appearance of national SI analytical standard, also will produce far reaching significance to testing agency's umpire analysis.
Description of drawings
The HPLC-ELSD canonical plotting of Fig. 1 SI.■ embodiment 1, ◆ embodiment 2.
The HPLC-ELSD test result spectrogram of SI among Fig. 2 Igepon A.
The HPLC-ELSD test result spectrogram of SI in the synthetic soap of Fig. 3.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
Experimental apparatus:
WATERS1525 type high performance liquid chromatograph (U.S. Waters);
Waters2420 type EISD (U.S. Waters);
The Empower chromatographic work station;
Ultrasonic cleaning machine, Shanghai High Kudos Science Instrument Co., Ltd.;
JA1004 electronic balance (1/10000 balance) (Shanghai Precision Scientific Apparatus Co., Ltd);
Dionex OnGuard II RP pre-treatment pre-column (U.S. Dionex);
Dionex 500 ion chromatographs (U.S. Dionex);
DionexAG11-AS11-HC separating column (U.S. Dionex);
Dionex electric conductivity detector (U.S. Dionex).
Chromatographic condition:
The stainless steel column of chromatographic column: 250mm * 4.6mm (id), Lichrospher-5 μ m-C
18Filler;
Moving phase is formed volume ratio: methyl alcohol: ultrapure water=100: 0;
Flow velocity: 0.4mL/min;
Column temperature: 25 ℃;
EISD;
Jet chamber's rank of detecting device: 60%;
Drift tube temperature: 50 ℃;
Nitrogen pressure: 20psi;
Sample size: 20 μ L.
Medicine:
Yi Jiebang A: technical grade, Yongan, Huang gang pharmaceutcal corporation, Ltd;
Isethionic acid sodium water solution (massfraction is 48%): technical grade (wherein active matter content massfraction >=99.1%), Yongan, Huang gang pharmaceutcal corporation, Ltd;
Commercially available synthetic soap;
Methyl alcohol: chromatographically pure, Chemical Reagent Co., Ltd., Sinopharm Group;
It is pure that other reagent are analysis.
Determination step:
1, the processing of standard items
Getting massfraction is that 48%SI WS 10mg adds the 100mL absolute ethyl alcohol, and water-bath is heated to transparent, puts into refrigerator (0～5 ℃); Behind the 12h; Treat that whole crystallizations separate out, suction filtration is also dry, and 105 ± 2 ℃ dry to constant weight and obtain SI powder (active matter quality mark >=99.1%).
2, the preparation of isethionic acid sodium standard solution
Accurately take by weighing the SI pressed powder 100.0mg that was handled by step 1. and place the 50mL volumetric flask, to scale, the SI mass concentration is 2.0mg/mL with methanol constant volume.
3, the preparation of Igepon A solution and synthetic soap sample solution
Accurately take by weighing Igepon A solid and each 50.0mg of synthetic soap, add 30mL methyl alcohol ultrasonic dissolution 1min respectively, move to respectively in the 100mL volumetric flask, and with methanol constant volume to scale.Mass concentration is 0.5mg/mL.With the nylon filter paper filtering of 0.20 μ m, clear liquid was for use before sample solution used.
4, chromatography of ions is with the preparation of sample solution
Take by weighing the SI pressed powder 23.749mg that was handled by step 1. and put into the 50mL beaker, add a small amount of ultrapure water dissolving, transfer in the 50mL volumetric flask, constant volume gets the SI standard solution that chromatography of ions is used, and mass concentration is 0.475mg/mL.Take by weighing the synthetic soap of 825mg Igepon A and 525mg, add the 30mL ultrapure water, great amount of bubbles appears in ultrasonic dissolution 5min, adds 2～3 absolute ethyl alcohols and is settled to 50mL behind the bubble clearly, and mass concentration is respectively 16.5mg/mL and 10.5mg/mL.
5, typical curve and linear relationship
SI standard solution in the accurate absorption step 2. places volumetric flask, methanol constant volume; Get the SI standard solution that mass concentration is respectively 0.004mg/mL, 0.02mg/mL, 0.04mg/mL, 0.08mg/mL, 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.6mg/mL, 0.8mg/mL and 1.0mg/mL, measure by above-mentioned chromatographic condition, every part of contrast liquid is measured 5 times; Get peak area mean value; With the massfraction is horizontal ordinate, and peak area is an ordinate, and getting typical curve is y=964348340.75x-1066624.69; The range of linearity is 0.004～1.0mg/mL, R
2=1.000 (shown in Figure 1).
6, the HPLC-ELSD method is measured the result
Igepon A and synthetic soap solution with step 3. preparation; Measure through the HPLC-ELSD method respectively; Calculate through typical curve: the mass concentration of SI is 0.01157mg/mL in Igepon A solution, and promptly the SI massfraction is 2.314% in Igepon A solid; The mass concentration of SI is 0.02090mg/mL in synthetic soap solution, and promptly the massfraction of SI is 4.180% in synthetic soap solid.
7, ion-chromatographic determination result
Through the chromatography of ions quantitative test, drawing the massfraction that contains SI among the Igepon A is 2.211%, and the massfraction that contains SI in the synthetic soap is 4.543% (seeing " the analytical test report " of Shanghai Organic Chemistry Institute, Chinese Academy of Sciences for details).Show that thus the HPLC-ELSD method measures the result and the ion-chromatographic determination result coincide.
8, the precision and recovery experiment
Getting mass concentration is 0.4mg/mL SI standard solution, repeats sample introduction 7 times, and gained mean value as a result is 0.385mg/mL, precision RSD 1.80%.
Accurately measuring 5 parts of mass concentrations is 0.1mg/mL Igepon A 2mL; Every part of 0mg/mL (blank), 0.004mg/mL, 0.02mg/mL, 0.04mg/mL, 0.08mg/mL SI standard solution that adds the 2mL volume measured respectively, gets 3 times and measures the mean value calculation recovery.The recovery 95.3～98.2%, the result sees table 1.Property makes an uproar than the concentration that is 3: 1 o'clock SI to be 0.02 μ g/mL, to be detection limit.It is thus clear that this method has good precision, reappearance and stability.
Table 1 recovery of standard addition calculates
| Amount/μ g before the mark-on | Addition/μ g | Amount/μ g behind the mark-on | Yield/μ g | The recovery/% |
| 0.023 | 0.04 | 0.063 | 0.061 | 96.8 |
| 0.023 | 0.20 | 0.223 | 0.219 | 98.2 |
| 0.023 | 0.40 | 0.423 | 0.403 | 95.3 |
| 0.023 | 0.80 | 0.823 | 0.792 | 96.2 |
In the table: the measured value * sample size of amount=blank mark-on solution quality concentration before the mark-on
Addition=standard solution mass concentration * sample size ÷ 2
Amount+addition before the amount=mark-on behind the mark-on
Measured value * the sample size of yield=mark-on solution quality concentration
Amount * 100% behind the recovery=yield ÷ mark-on
Embodiment 2
Chromatographic condition:
The stainless steel column of chromatographic column: 250mm * 4.6mm (id), Lichrospher-5 μ m-C
18Filler;
Moving phase is formed volume ratio: methyl alcohol: ultrapure water=100: 0;
Flow velocity: 0.8mL/min;
Column temperature: 25 ℃;
EISD;
Jet chamber's rank of detecting device: 60%;
Drift tube temperature: 40 ℃;
Nitrogen pressure: 20psi;
Sample size is 20 μ L.
All the other embodiments are all identical with embodiment 1.
1, typical curve and linear relationship
The accurate SI standard solution of drawing in embodiment 1 step 2 places volumetric flask, methanol constant volume; Get the SI standard solution that mass concentration is respectively 0.004mg/mL, 0.02mg/mL, 0.04mg/mL, 0.08mg/mL, 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.6mg/mL, 0.8mg/mL and 1.0mg/mL, measure by above-mentioned chromatographic condition, every part of contrast liquid is measured 5 times; Get peak area mean value; With the massfraction is horizontal ordinate, and peak area is an ordinate, and getting typical curve is y=718740358.37x+185333.11; The range of linearity is 0.004～1.0mg/mL, R
2=0.995 (shown in Figure 1).
Because the difference of the operating conditionss such as flow velocity of liquid chromatography, gained typical curve also can be different.
2, the HPLC-ELSD method is measured the result
The Igepon A and the synthetic soap solution of the preparation of embodiment 1 step 3.; Measure through the HPLC-ELSD method; Calculate through typical curve: the mass concentration of SI is 0.01193mg/mL in Igepon A solution, and promptly the SI massfraction is 2.386% in Igepon A solid; The mass concentration of SI is 0.02047mg/mL in synthetic soap solution, and promptly the massfraction of SI is 4.094% in synthetic soap solid.Identical basically with the ion chromatography result.
3, the precision and recovery experiment
Getting mass concentration is 0.4mg/mL SI standard solution, repeats sample introduction 7 times, and gained mean value as a result is 0.380mg/mL, precision RSD 2.65%.
Accurately measuring 5 parts of mass concentrations is 0.1mg/mL Igepon A 2mL; Every part of 0mg/mL (blank), 0.004mg/mL, 0.02mg/mL, 0.04mg/mL, 0.08mg/mL SI standard solution that adds the 2mL volume measured respectively, gets 3 times and measures the mean value calculation recovery.The recovery 95.2%～98.3%, the result sees table 2.
Table 2 recovery of standard addition calculates
| Amount/μ g before the mark-on | Addition/μ g | Amount/μ g behind the mark-on | Yield/μ g | The recovery/% |
| 0.023 | 0.04 | 0.063 | 0.060 | 95.2 |
| 0.023 | 0.20 | 0.223 | 0.215 | 96.4 |
| 0.023 | 0.40 | 0.423 | 0.416 | 98.3 |
| 0.023 | 0.80 | 0.823 | 0.789 | 95.8 |
In the table: the measured value * sample size of amount=blank mark-on solution quality concentration before the mark-on
Addition=standard solution mass concentration * sample size ÷ 2
Amount+addition before the amount=mark-on behind the mark-on
Measured value * the sample size of yield=mark-on solution quality concentration
Amount * 100% behind the recovery=yield ÷ mark-on
Claims (3)
1. the HPLC analytical method of a sodium isethionate SI is characterized in that adopting high performance liquid chromatography, cooperates EISD, measures the content of SI with calibration curve method; The high performance liquid chromatography operating conditions is:
The stainless steel column of chromatographic column: 250mm * 4.6mm, Lichrospher-5 μ m-C
18Filler;
Moving phase is formed volume ratio: methyl alcohol: ultrapure water=100: 0;
Flow velocity: 0.2～1.2mL/min;
Column temperature: 25 ℃;
Detecting device: EISD;
Jet chamber's rank 50%～80% of detecting device;
40～60 ℃ of drift tube temperatures;
Nitrogen pressure 15～40psi;
Sample size is 20 μ L;
Reference material: adopt the SI powder of >=99% purity or the SI WS of massfraction 48%.
2. according to the HPLC analytical method of the said SI of claim 1, it is characterized in that:
Moving phase is formed volume ratio: methyl alcohol: ultrapure water=100～80: 0～20;
Flow velocity: 0.3～0.8mL/min;
Column temperature: 25～50 ℃;
Jet chamber's rank of detecting device is 60%;
40～50 ℃ of drift tube temperatures;
Nitrogen pressure 20psi;
Reference material: the SI powder that adopts >=99% purity.
3. according to the HPLC analytical method of claim 1 or 2 said SI, it is characterized in that: described moving phase is used ultrasonic degas before use.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077739A (en) * | 1992-03-20 | 1993-10-27 | 普罗格特-甘布尔公司 | Cleansing bar with skin pH value |
| EP1479377A1 (en) * | 2003-05-22 | 2004-11-24 | Unilever Plc | Personal product bar compositions comprising crystalline wax structured pre-mix or delivery vehicle |
| EP1582579A2 (en) * | 2004-03-29 | 2005-10-05 | Nippon Shokubai Co., Ltd. | Detergent and fabric care additive containing carboxylic acid polymer |
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2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077739A (en) * | 1992-03-20 | 1993-10-27 | 普罗格特-甘布尔公司 | Cleansing bar with skin pH value |
| EP1479377A1 (en) * | 2003-05-22 | 2004-11-24 | Unilever Plc | Personal product bar compositions comprising crystalline wax structured pre-mix or delivery vehicle |
| EP1582579A2 (en) * | 2004-03-29 | 2005-10-05 | Nippon Shokubai Co., Ltd. | Detergent and fabric care additive containing carboxylic acid polymer |
Non-Patent Citations (2)
| Title |
|---|
| 徐宝财 等.脂肪酰氧乙基磺酸盐类表面活性剂的研究进展.《现代化工增刊(2)》.2008,第28卷366-368. * |
| 薛晓义 等.椰油酰基羟乙基磺酸钠的性能和应用研究.《2004(第八届)国际表面活性剂和洗涤剂会议论文集》.2004,173-176. * |
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