CN106442771A - Detection method for determining sodium tetradecyl sulfate and related substances thereof - Google Patents
Detection method for determining sodium tetradecyl sulfate and related substances thereof Download PDFInfo
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Abstract
The invention discloses a detection method for determining sodium tetradecyl sulfate and related substances thereof. The detection method is a high performance liquid chromatography-evaporation light scattering method, wherein a water-organic solvent with the volume ratio ranging from (30 : 70) to (10 : 90) is used as a solvent to prepare a solution of a sample to be tested; for high performance liquid chromatography, an isocratic elution manner is adopted to carry out elution; chromatographic conditions are as follows: an immobile phase is an octadecyl bonded silica gel chromatographic column, a mobile phase is a water phase-organic phase system, the pH (Potential of Hydrogen) of a water phase is 3.0 to 6.0, and the volume ratio of the water phase to an organic phase ranges from (30 : 70) to (5 : 95), wherein the temperature of a drift tube of a detector for evaporation light scattering is 30 DEG C to 80 DEG C, and gas-carrying pressure is 20psi to 45psi. The detection method provided by the invention has the characteristics of good separation degree, simplicity and rapidness, high specificity, high sensitivity and the like.
Description
Technical field
The present invention relates to pharmaceutical analysiss detection field is and in particular to a kind of measure sodium tetradecyl sulfate and its relevant material
Detection method.
Background technology
Sodium tetradecyl sulfate (sodium tetradecyl sulphate, STDS) is a kind of branched alkane of chemosynthesis
Base anion surfactant, is mainly used in wetting agent and transdermal enhancer in pharmaceutical preparation, also can be as sclerosing agent to control
Treat varicose veins of the lower extremity.Its chemical entitled Sodium 4-Ethyl-1-iobutyoctylsulohate, molecular formula is C14H29O4SNa, chemistry knot
Structure is as follows：
Sodium tetradecyl sulfate no ultraviolet absorption group, soluble in water, unstable chemcial property, in illumination, high temperature or pole
Easily degrade under the pH environment of end.In product is mainly 4- ethyl -1- isobutyl group octane alcohol about material, and water solublity is poor.Two
The difference of person's physics and chemical property causes difficulty to separating analysis.And in medicine preparation and storage process, main constituent is contained
Amount, process contaminants and degradation impurity are fast and accurately detected, for the quality production process of finished product and the quality of medicine
Control particularly significant.
At present, the open method of the content for sodium tetradecyl sulfate and the detection of relevant material is detected in British Pharmacopoeia
2015 editions.Wherein, the relevant material of crude drug adopts the gas chromatography after n-hexane extraction, and the response rate is easily subject to pre-treatment shadow
Ring, and the no corresponding detection of its injection.Content detection adopts direct diphasic titration, that is, in the two-phase medium of chloroform and water
With bromination bottom rice as indicator, with the titration of benzyl chloride Soviet Union to determine the concentration of sulfate anion surfactant.This method
Lack specificity, titration results are easily disturbed by other alkyl sulfide acids surfactants.
Additionally, the standard detection of sulphuric acid analog anion surfactants mainly adopts titrimetry, such as GB GB/T 5173-
1995《The direct diphasic titration of mensure of surfactant and detergent Anionic Active》.(the dodecyl sulfur such as Liu Jianzhen
Sour sodium quality controling research, pharmaceutical analysiss magazine [J], 2009 (7)) by the water of gas chromatography mensure sodium lauryl sulphate
Solution product dodecanol is to determine content.Though the method can detect the content of main constituent homologue impurity, mask original
The impurity content of lauryl alcohol.Chinese patent literature CN101576481A adopt sub-methyl blue spectrum analysis measure alkali metal salt,
Contents of anionic surface active substances in the hydroxide of alkali salt and alkaline-earth metal.Chinese patent literature
CN101308121A adopts the sulfonic acid analog anion surfactants through multistep pre-treatment for the GC-MS detection, and is not directed to sulfuric acid
Anion surfactant.Yuan Chunli etc. (chromatography of ions detection anion surfactant, resources conservation and environmental protection [J], 2013
(5) the n-tetradecane base sodium sulfate in chromatography of ions-Suppressor conductivity detection method analysis environments water body and its homologue) are established,
And relevant material (including intermediate, the by-product and catabolite) detection for sulphuric acid analog anion surfactants then has no
Report.
Content of the invention
The technical problem to be solved is to overcome the content detection of sodium tetradecyl sulfate of the prior art
Mainly adopt titrimetry, there is lacking of specificity poor (titrimetry cannot exclude the interference of other chain alkyl sodium sulfate homologues)
Fall into and sodium tetradecyl sulfate relevant material detection mainly adopt gas chromatography, exist the response rate easily affected by pre-treatment,
The not high defect of accuracy, and provide a kind of mensure sodium tetradecyl sulfate and its detection method about material.The present invention
The detection method providing has the features such as separating degree is good, simple and quick, specificity is strong, sensitivity is high, can be used for myristyl sulfur
The quality evaluation of process quality control and finished product in sour sodium raw materials medicine synthesis technique and preparation process.
The invention provides a kind of mensure sodium tetradecyl sulfate and its detection method about material, described detection side
Method is HPLC ELSD method, wherein, with volume ratio for (30:70)～(10:90) water-organic solvent is
Need testing solution prepared by solvent, and high performance liquid chromatography carries out eluting using isocratic elution mode, and its chromatographic condition is：Fixing phase is
Octadecyl silane chromatographic column, mobile phase is aqueous phase-organic phase system, and the pH of aqueous phase is 3.0～6.0, aqueous phase with organic
The volume ratio of phase is (30:70)～(5：95)；Wherein, the drift tube temperature of the detector that evaporat light scattering uses is 30～80
DEG C, nebulizer gas pressure is 20～45psi.
In the present invention, described sodium tetradecyl sulfate, in the case of clearly not distinguishing, can be that 4- ethyl -1- is different
The sterling of butyl octyl sodium sulfate, crude drug or preparation etc. are using Sodium 4-Ethyl-1-iobutyoctylsulohate as main constituent
Product.The assay method of the present invention is all applied to the quality control of the said goods, and the survey of the relevant material of these products
Determine method also within the scope of the present invention.
In the present invention, described relevant material refers in medicine preparation and storage process, it is understood that there may be initiation material,
Intermediate, polymer, side reaction product and degradation impurity.Described intermediate refers to that in building-up process, extraction washes before refining 14
Alkyl sodium sulfate crude product, is the mixture of sodium tetradecyl sulfate, reaction residue and other by-products.
In the present invention, the organic solvent prepared in the solvent of need testing solution is preferably acetonitrile, methanol or ethanol；Prepare
The solvent of need testing solution is 15 more preferably for volume ratio:85 water-acetonitrile.
In the present invention, described aqueous phase is the aqueous phase of the conventional chromatogram analysis method in this area, is preferably comprised water, organic
One or more of aqueous acid, buffer salt solution, more preferably for buffer salt solution.In wherein said aqueous solutions of organic acids
Organic acid be preferably formic acid and/or acetic acid, the salt in described buffer salt solution be preferably ammonium formate, ammonium acetate, carbon
One or more of sour ammonium, more preferably for ammonium acetate.The concentration of described aqueous solutions of organic acids preferably 0.01mol/L～
0.20mol/L.The concentration of described buffer salt solution is preferably 0.01mol/L～0.20mol/L, more preferably for 0.05～
0.10mol/L, is more preferably 0.10mol/L further；PH value is preferably 5.8.
In the present invention, described organic faciess are the conventional solvent or the solution that are applied to chromatogram analysis method in this area, relatively
Include one or more of methanol, ethanol, acetonitrile, more preferably for methanol and/or acetonitrile goodly.It is preferred that described aqueous phase-have
Aqueous phase in machine phase system is water, and organic faciess are acetonitrile.
In the present invention, described aqueous phase is preferably (20 with the volume ratio of described organic faciess:80)～(5：95), more preferably for
15:85.
In the present invention, the flow velocity of described mobile phase is this area normal condition, preferably 0.5mL/min～1.5mL/
Min, more preferably for 1.0mL/min.
In the present invention, the condition that described octadecyl silane chromatographic column is adopted is this area normal condition, described
Preferably 3-5 μm of the filler particles degree of octadecyl silane chromatographic column, more preferably for 3 μm；Described octadecyl bonding
Preferably 20～40 DEG C of the column temperature of silica gel chromatographic column, more preferably for 30 DEG C；The entering of described octadecyl silane chromatographic column
Sample volume is preferably 0.1～100 μ L.
In the present invention, during being evaporated scattering measuring, it is preferred that also low-temperature atomizing is carried out to detection sample.
In the present invention, preferably 50 DEG C of the drift tube temperature of the detector that evaporat light scattering uses, nebulizer gas pressure is preferable
Ground is 30.0psi.
In the present invention one better embodiment, provide uses the tablets by HPLC-ELSD tetradecane
Base sodium sulphate content and the method about material, specifically include following steps：
A. weigh sodium tetradecyl sulfate reference substance appropriate, be placed in volumetric flask, with water-acetonitrile (15:85) dissolving and dilute
Release to scale, the concentration obtaining sodium tetradecyl sulfate is the solution of 3mg/mL, as reference substance solution A.From reference substance solution A
In take and be respectively placed in right amount in volumetric flask, be configured to a series of reference substance solution B that concentration is respectively 6 μ g/mL～600 μ g/mL；
B. take sodium tetradecyl sulfate test sample appropriate, with water-acetonitrile (15:85) it is configured to concentration for solvent to be respectively
The need testing solution B of the need testing solution A of 3.0～6.0mg/mL and 0.3～0.6mg/mL；
C. take a series of reference substance solution B in step a, each 10 μ L sample introductions of need testing solution A and need testing solution B, adopt
With the detection of HPLC ELSD method, drawn according to reference substance solution main peak peak area and reference substance solution concentration
Double-log standard curve.In test sample, main constituent or the content about material substitute into calibration curve equation meter by the peak area recording
Obtain.
On the basis of meeting common sense in the field, above-mentioned each optimum condition, can combination in any, obtain final product each preferable reality of the present invention
Example.
Agents useful for same of the present invention and raw material are all commercially available.
The positive effect of the present invention is：The method of the present invention has that separating degree is good, simple and quick, specificity strong,
The features such as sensitivity is high, it is applied to the detection of sodium tetradecyl sulfate and its intermediate impurities, can be used for 4- ethyl -1- isobutyl
The qualitative and quantitative analysis of base octane alcohol, sodium tetradecyl sulfate and its intermediate, or be further used for monitoring myristyl sulfur
The quality of sour sodium synthesis process, finished product or crude drug and preparation.
Brief description
Fig. 1 is the HPLC of sodium tetradecyl sulfate and 4- ethyl -1- isobutyl group octane alcohol mixing reference substance in embodiment 1
Figure；
Fig. 2 is the HPLC complete graph of sodium tetradecyl sulfate relevant material detection in embodiment 1；
Fig. 3 is the HPLC partial enlarged drawing of sodium tetradecyl sulfate relevant material detection in embodiment 1；
Fig. 4 is the HPLC figure of sodium tetradecyl sulfate synthetic intermediate detection in embodiment 2；
Fig. 5 is the HPLC figure of sodium tetradecyl sulfate content detection in embodiment 3；
Fig. 6 is the HPLC figure of sodium tetradecyl sulfate injection content detection in embodiment 4；
Fig. 7 is the forced degradation test HPLC complete graph of sodium tetradecyl sulfate crude drug in embodiment 5；
Fig. 8 is the forced degradation test HPLC partial enlarged drawing of sodium tetradecyl sulfate crude drug in embodiment 5.
Specific embodiment
Further illustrate the present invention below by the mode of embodiment, but therefore do not limit the present invention to described reality
Apply among a scope.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or according to business
Product description selects.
In following embodiments, the source of product and model are as follows：
Methanol, acetonitrile, ethanol are HPLC level, purchased from Fisher company；
Formic acid, acetic acid are HPLC level, purchased from Fluka company；
Ammonium formate is AR level, purchased from Chemical Reagent Co., Ltd., Sinopharm Group；
Ammonium carbonate is AR level, purchased from Chemical Reagent Co., Ltd., Sinopharm Group；
Ammonium acetate is AR level, purchased from Chemical Reagent Co., Ltd., Sinopharm Group；
Sodium tetradecyl sulfate reference substance is purchased from Shanghai Zi Yuan Pharmaceutical, lot number S141204；
4- ethyl -1- isobutyl group octane alcohol reference substance is purchased from ladder uncommon love (Shanghai) chemical conversion industry Development Co., Ltd (TCI),
Lot number FIM03-QQHL；
Sodium tetradecyl sulfate injection is purchased from Mylan company of the U.S., lot number 150322.
In following embodiments, the source of the instrument being used and model are as follows：
High performance liquid chromatograph：Model Alliance e2695, purchased from water generation science and technology (Shanghai) Co., Ltd.
(Waters)；
Evaporative light scattering detector：Model 2424 type, purchased from water generation science and technology (Shanghai) Co., Ltd.；
Octadecyl silane chromatographic column：For Acclaim Surfactant chromatographic column.
In following embodiments, the data processing software being used is as follows：Empower 3 data handling system.
Embodiment 1
The present embodiment is the relevant material detection embodiment of sodium tetradecyl sulfate.
Experiment condition is as follows：
Acclaim Surfactant chromatographic column (5 μm of filler particles degree, 4.6 × 150mm).Mobile phase is 0.10mol/L
Formic acid aqueous ammonium-acetonitrile (volume ratio 15:85, with first acid for adjusting pH to 4.7), flow velocity 1.0mL/min, 25 DEG C of column temperature.Detection
70 DEG C of device drift tube temperature, low-temperature atomizing, nebulizer gas pressure 30.0psi, gain 100.
Experimental procedure is as follows：
Take sodium tetradecyl sulfate reference substance 3mg, 4- ethyl -1- isobutyl group octane alcohol reference substance 10 μ L respectively, with water-second
Nitrile (volume ratio 15:85) it is configured to system suitability solution for solvent, takes 10 μ L sample introductions, dissipated with high performance liquid chromatography-evaporative light
The method of penetrating is detected, obtains spectrogram 1.Precision weighs sodium tetradecyl sulfate reference substance 60mg, is placed in 20mL volumetric flask, with
Water-acetonitrile (15:85) dissolve and be diluted to scale for solvent, that is, the concentration obtaining sodium tetradecyl sulfate is the molten of 3mg/mL
Liquid, draws this mother solution 20 μ L, 100 μ L, 200 μ L, 300 μ L, 500 μ L are respectively placed in 10mL volumetric flask, with water-acetonitrile (15:
85) be solvent dilution to scale as reference substance solution, take 10 μ L sample introductions, carried out with HPLC ELSD method
Detection, draws double-log standard curve according to a series of reference substance solution main peak peak areas and reference substance solution concentration.Accurate title
Take 30mg testing sample, be placed in 10mL volumetric flask, with water-acetonitrile (15:85) dissolve for solvent and be diluted to scale, take above-mentioned
Solution 10 μ L sample introduction, is detected with HPLC ELSD method, obtain spectrogram 2, its enlarged drawing is as shown in Figure 3.
Sample main peak area is substituted into the content that calibration curve equation calculates intermediate.
As shown in figure 1, being sodium tetradecyl sulfate and 4- ethyl -1- isobutyl group octane alcohol mixing reference substance in the present embodiment
HPLC figure, wherein the retention time of sodium tetradecyl sulfate be 5.673min, during the reservation of 4- ethyl -1- isobutyl group octane alcohol
Between be 3.403min, the two baseline separation.Fig. 2,3 be respectively sodium tetradecyl sulfate relevant material detection HPLC complete graphs,
Partial enlarged drawing.In Fig. 1 and Fig. 2 (or Fig. 3), the peak of retention time respectively 2.108min, 2.141min is myristyl sulfur
Sodium ion peak in sour sodium.In Fig. 2 and Fig. 3, except sodium tetradecyl sulfate (retention time is 5.623min), 4- ethyl -1- are different
Butyl octane alcohol (retention time is 3.386min) outward, also detects two unknown impurities, baseline separation between each peak, this is described
Bright detection method separating degree is good.It is computed, the content about 4- ethyl -1- isobutyl group octane alcohol in material is 0.37%, always
Impurity content is 4.0%, and described percentage ratio is mass percent.
Embodiment 2
The present embodiment is the purity detecting embodiment of sodium tetradecyl sulfate synthetic intermediate.
Experiment condition is as follows：
Acclaim Surfactant chromatographic column (5 μm of filler particles degree, 4.6 × 150mm).Mobile phase is 0.05mol/L
Ammonium acetate solution-acetonitrile (volume ratio 15:85, with second acid for adjusting pH to 5.8), flow velocity 1.0mL/min, 30 DEG C of column temperature.Detection
50 DEG C of device drift tube temperature, low-temperature atomizing, nebulizer gas pressure 30.0psi, gain 100.
Experimental procedure is as follows：
Precision weighs sodium tetradecyl sulfate reference substance 60mg, is placed in 20mL volumetric flask, with water-acetonitrile (volume ratio 20:
80) dissolve for solvent and be diluted to scale, draw this mother solution 800 μ L, 1000 μ L, 1200 μ L are respectively placed in 10mL volumetric flask,
With water-acetonitrile (20:80) for solvent dilution to scale, as comparison liquid.Precision measures 140 μ L midbody solutions, is placed in 10mL
In volumetric flask, with water-acetonitrile (20:80) dissolve for solvent and be diluted to scale, as test liquid.The each 10 μ L of above-mentioned solution are taken to enter
Sample, calculates the content of intermediate with standard curve method.
As can be seen that sodium tetradecyl sulfate and 4- ethyl -1- isobutyl group octane alcohol mixing reference substance from embodiment 1
In spectrogram, three peaks are respectively sodium ion peak, 4- ethyl -1- isobutyl group octane alcohol and sodium tetradecyl sulfate peak, accordingly, just
The absworption peak that can judge 3.065min in Fig. 4 is also 4- ethyl -1- isobutyl group octane alcohol, also because the angle from synthesis chemistry is divided
Analysis, 4- ethyl -1- isobutyl group octane alcohol is reactant, is also major degradants.
I.e. in Fig. 4, the retention time of sodium tetradecyl sulfate is 4.837min, and the retention time of residual reactants is
3.065min, the two baseline separation, the peak of 2.144min is the sodium ion peak in sodium tetradecyl sulfate.Regression equation is y=
1.4237x+7.1227, R2=0.9999.It is computed, this intermediates content is 97.8%.
Embodiment 3
The present embodiment is the content detection embodiment of sodium tetradecyl sulfate.
Experiment condition is as follows：
Tested using experiment condition similar to Example 2 and step, be the difference is that only：Wherein in mobile phase
Aqueous phase be replaced by the 0.10mol/L ammonium acetate solution of pH 5.5, the compound method of need testing solution is replaced by precision and weighs
30mg sample, is placed in 100mL volumetric flask, with water-acetonitrile (15:85) dissolve for solvent and be diluted to scale.
As shown in figure 5, the retention time of sodium tetradecyl sulfate is 4.813min.Main peak and other impurities peak A are (during reservation
Between 3.021min) separating degree good.Regression equation is y=1.4415x+6.9929, R2=0.9998.It is computed, the tetradecane
The content of base sodium sulfate is 100.3%.In Fig. 5, the peak of 2.151min is the sodium ion peak in sodium tetradecyl sulfate,
3.021min is impurity peaks, and the main component of impurity is also 4- ethyl -1- isobutyl group octane alcohol.
Embodiment 4
The present embodiment is the content detection embodiment of sodium tetradecyl sulfate injection.
Experiment condition is as follows：
Tested using experiment condition similar to Example 2 and step, wherein the aqueous phase in mobile phase is replaced by
0.05mol/L ammonium carbonate solution, mobile phase is that (volume ratio is 22 to 0.05mol/L ammonium carbonate solution-acetonitrile:78, with formic acid
Adjust pH to 4.1), the compound method of need testing solution is replaced by precision and measures 1mL sample, is placed in 10mL volumetric flask, with water-
Acetonitrile (15:85) dissolve and be diluted to scale for solvent, detector nebulizer gas pressure is replaced by 40psi.
As shown in fig. 6, the retention time of sodium tetradecyl sulfate is 6.284min.Main peak and other impurities peak A are (during reservation
Between 3.614min) separating degree good.Regression equation is y=1.4368x+7.3548, R2=0.9998.It is computed, the tetradecane
The content of base sulphuric acid sodium injection is 105.4%.In Fig. 6, in addition to sodium tetradecyl sulfate main peak, other two peaks are respectively：
The peak of 2.068min is the sodium ion peak in sodium tetradecyl sulfate, and 3.614min is impurity peaks.
Embodiment 5 specificity is tested
Experiment condition is as follows：
Tested using experiment condition similar to Example 2 and step, wherein the aqueous phase in mobile phase be replaced by dense
Spend for 0.10mol/L ammonium acetate solution, mobile phase is ammonium acetate solution-acetonitrile (volume ratio 15:85), need testing solution
Compound method is replaced by precision and weighs five parts of 45mg sample, is placed in 100mL volumetric flask, with water-acetonitrile (15:85) it is that solvent is molten
Solution, wherein three parts are separately added into appropriate hydrochloric acid, sodium hydroxide solution, hydrogen peroxide, after being diluted to scale 40 DEG C of decentralizations set to 0 .5～
3h；After another two parts are diluted to scale, portion is placed in 105 DEG C of 3h after taking appropriate sealing, and another is placed in strong illumination lower 7 days.
As shown in Figure 7, Figure 8, experiment condition from top to bottom is followed successively by acid, alkali, oxidation, heat, photo damage.Myristyl sulfur
Sour sodium (retention time about 4.72min) is good with the separating degree at each degradation impurity peak, and the detection method specificity of the present invention is described
By force.In Fig. 7, Fig. 8, the peak of about 2.1min is sodium ion peak, and in first in Fig. 7 and Fig. 8 component, the peak of about 3.0min is
The chloride ion peak of hydrochloric acid.Additionally, other peaks are degradation impurity peak.
Embodiment 6 precision test
Experiment condition is as follows：
Tested using experiment condition similar to Example 5 and step, precision weighs sodium tetradecyl sulfate comparison
Appropriate product, with water-acetonitrile (15:85) dissolve for solvent, be configured to each 6 parts of the solution of 0.3mg/mL and 0.03mg/mL.Connect successively
Continuous sample introduction test, the main peak peak area RSD of 6 parts of 0.3mg/mL solution is 1.50%, the main peak peak face of 6 parts of 0.03mg/mL solution
Long-pending RSD is 1.85%.Result shows, this method is respectively provided with good precision under high and low concentration.
Embodiment 7 sensitivity test
Experiment condition is as follows：
Tested using experiment condition similar to Example 4 and step, precision weighs sodium tetradecyl sulfate comparison
Appropriate product, with water-acetonitrile (15:85) dissolve for solvent, be configured to 3 parts of the solution of 6 μ g/mL.Sampling volume 20 μ L.Chromatographic results
It is shown in Table 1.The detection method of the present invention is limited to 60ng for the quantitation of sodium tetradecyl sulfate.Result shows, this method is after testing
Sensitivity is fine.
The effect data of table 1 embodiment 7
Embodiment 8
In the present embodiment, carry out the content of sodium tetradecyl sulfate using experiment condition similar to Example 3 and step
Detection, the difference is that only：The organic solvent prepared in the solvent of need testing solution is methanol, the body of water and methanol in solvent
Long-pending ratio is 30:70；In mobile phase, aqueous phase is the aqueous formic acid of pH3.0, and aqueous phase is 30 with the volume ratio of organic faciess:70；Evaporation
The drift tube temperature of the detector that light scattering uses is 30 DEG C, and nebulizer gas pressure is 45psi.
The present embodiment also can obtain baseline separation similar to Example 3 clearly spectrogram.
Embodiment 9
In the present embodiment, carry out the content of sodium tetradecyl sulfate using experiment condition similar to Example 3 and step
Detection, the difference is that only：The organic solvent prepared in the solvent of need testing solution is ethanol, the body of water and ethanol in solvent
Long-pending ratio is 10:90；In mobile phase, aqueous phase is the aqueous formic acid of pH3.0, and aqueous phase is 5 with the volume ratio of organic faciess:95；Evaporation
The drift tube temperature of the detector that light scattering uses is 80 DEG C, and nebulizer gas pressure is 20psi.
The present embodiment also can obtain baseline separation similar to Example 3 clearly spectrogram.
Claims (10)
1. a kind of measure sodium tetradecyl sulfate and its about material detection method it is characterised in that described detection method
For HPLC ELSD method, wherein, with volume ratio for (30:70)～(10:90) water-organic solvent is molten
Need testing solution is prepared in agent, and high performance liquid chromatography carries out eluting using isocratic elution mode, and its chromatographic condition is：Fixing phase is ten
Eight alkyl linked silica gel chromatographic columns, mobile phase is aqueous phase-organic phase system, and the pH of aqueous phase is 3.0～6.0, aqueous phase and organic faciess
Volume ratio be (30:70)～(5：95)；Wherein, the drift tube temperature of the detector that evaporat light scattering uses is 30～80 DEG C,
Nebulizer gas pressure is 20～45psi.
2. detection method as claimed in claim 1 is it is characterised in that the organic solvent in the solvent of preparation need testing solution is
Acetonitrile, methanol or ethanol.
3. detection method as claimed in claim 2 is it is characterised in that the solvent preparing need testing solution is 15 for volume ratio:
85 water-acetonitrile.
4. detection method as claimed in claim 1 is it is characterised in that described aqueous phase includes water, aqueous solutions of organic acids, buffering
One or more of saline solution.
5. detection method as claimed in claim 4 is it is characterised in that the organic acid in described aqueous solutions of organic acids is formic acid
And/or acetic acid；The concentration of described aqueous solutions of organic acids is 0.01mol/L～0.20mol/L；In described buffer salt solution
Salt is one or more of ammonium formate, ammonium acetate, ammonium carbonate；The concentration of described buffer salt solution be 0.01mol/L～
0.20mol/L, pH are 5.8.
6. detection method as claimed in claim 5 it is characterised in that the concentration of described buffer salt solution be 0.05～
0.10mol/L.
7. detection method as claimed in claim 1 it is characterised in that described organic faciess include methanol, ethanol, in acetonitrile
One or more；Described aqueous phase is (20 with the volume ratio of described organic faciess:80)～(5：95).
8. detection method as claimed in claim 7 is it is characterised in that described aqueous phase is 15 with the volume ratio of described organic faciess:
85.
9. detection method as claimed in claim 1 it is characterised in that described mobile phase flow velocity be 0.5mL/min～
1.5mL/min；The filler particles degree of described octadecyl silane chromatographic column is 3-5 μm；Described octadecyl silane
The column temperature of chromatographic column is 20～40 DEG C；The sampling volume of described octadecyl silane chromatographic column is 0.1～100 μ L；Evaporation
The drift tube temperature of the detector that light scattering uses is 50 DEG C, and nebulizer gas pressure is 30.0psi.
10. detection method as claimed in claim 9 is it is characterised in that the flow velocity of described mobile phase is 1.0mL/min；Described
The column temperature of octadecyl silane chromatographic column is 30 DEG C；During being evaporated scattering measuring, also detection sample is entered
Row low-temperature atomizing.
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| CN108072718A (en) * | 2018-02-09 | 2018-05-25 | 西北大学 | A kind of method that high performance liquid chromatography measures MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride content |
| CN109254087A (en) * | 2017-06-20 | 2019-01-22 | 海南先声药业有限公司 | A kind of HPLC detection method of lauryl sodium sulfate in Ezetimibe piece sample |
| CN109254086A (en) * | 2017-06-20 | 2019-01-22 | 海南先声药业有限公司 | A kind of HPLC detection method of lauryl sodium sulfate in cefaclor dry suspensoid sample |
| CN109541070A (en) * | 2018-12-20 | 2019-03-29 | 上海开米科技有限公司 | A kind of remaining method of detergent on liquid chromatographic detection fabric |
| CN111983043A (en) * | 2019-05-22 | 2020-11-24 | 天士力生物医药股份有限公司 | Method for detecting poloxamer residual quantity in recombinant human prourokinase raw material for injection |
| CN113341035A (en) * | 2021-07-29 | 2021-09-03 | 湖南沁森高科新材料有限公司 | Detection method of camphorsulfonic acid and sodium dodecyl sulfate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101308121A (en) * | 2007-05-14 | 2008-11-19 | 袁慧娟 | Sulfonic acid analog anion surfactants rapid checking method |
| CN101576481A (en) * | 2009-04-08 | 2009-11-11 | 中国科学院青海盐湖研究所 | Method for measuring contents of anionic surface active substances by methylene blue spectrometry |
-
2016
- 2016-09-05 CN CN201610802880.3A patent/CN106442771B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101308121A (en) * | 2007-05-14 | 2008-11-19 | 袁慧娟 | Sulfonic acid analog anion surfactants rapid checking method |
| CN101576481A (en) * | 2009-04-08 | 2009-11-11 | 中国科学院青海盐湖研究所 | Method for measuring contents of anionic surface active substances by methylene blue spectrometry |
Non-Patent Citations (3)
| Title |
|---|
| YUKIHIRO KONDOH: "Analysis of anionic surfactants by high performance liquid chromatography with conductive detector", 《油化学》 * |
| 杨敏 等: "高效液相色谱法测定依捷邦A产品中羟乙基磺酸钠的含量", 《日用化学工业》 * |
| 陈玉娥 等: "高效液相色谱法分析AES中的十二烷基硫酸钠", 《中国洗涤用品工业》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109254087A (en) * | 2017-06-20 | 2019-01-22 | 海南先声药业有限公司 | A kind of HPLC detection method of lauryl sodium sulfate in Ezetimibe piece sample |
| CN109254086A (en) * | 2017-06-20 | 2019-01-22 | 海南先声药业有限公司 | A kind of HPLC detection method of lauryl sodium sulfate in cefaclor dry suspensoid sample |
| CN108072718A (en) * | 2018-02-09 | 2018-05-25 | 西北大学 | A kind of method that high performance liquid chromatography measures MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride content |
| CN109541070A (en) * | 2018-12-20 | 2019-03-29 | 上海开米科技有限公司 | A kind of remaining method of detergent on liquid chromatographic detection fabric |
| CN111983043A (en) * | 2019-05-22 | 2020-11-24 | 天士力生物医药股份有限公司 | Method for detecting poloxamer residual quantity in recombinant human prourokinase raw material for injection |
| CN113341035A (en) * | 2021-07-29 | 2021-09-03 | 湖南沁森高科新材料有限公司 | Detection method of camphorsulfonic acid and sodium dodecyl sulfate |
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