CN102128909B - Method for separately identifying hybrid, single-chain and double-chain quaternary ammonium salts in disinfectant - Google Patents
Method for separately identifying hybrid, single-chain and double-chain quaternary ammonium salts in disinfectant Download PDFInfo
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Abstract
The invention discloses a method for separately identifying hybrid, single-chain and double-chain quaternary ammonium salts in disinfectant, which comprises the following steps: 1) sucking a solution to be detected and dipping on a silica gel G thin layered plate; 2) using the (the lower layer of chloroform-water solution)-methanol as a developer, adding a thick ammonia reagent solution in the other channel of a double-channel delaminating jar, pre-balancing and then delaminating; and 3) taking out, airing, fumigating with iodine steam, and then viewing in sunlight. The method is simple to operate and has the advantages of low cost and low requirements for instruments and equipment, and the like, and especially, the method can be used for efficiently avoiding the interference on an identifying result caused by other components in a quaternary ammonium salt-glutaraldehyde compound preparation, and the method is suitable for popularizing.
Description
Technical field
The invention belongs to the field is differentiated in the separation of compound in the chemicals, relate to a kind of method of differentiating bundle, strand and double-chain quaternary ammonium salt in the sanitizer of separating, be applied in the quality control detection to the compound quaternary ammonium salt sanitizer.
Background technology
The compound quaternary ammonium salt disinfectant for animals has advantages such as wide spectrum, efficient, low toxicity; Become present most widely used sanitizer; Wherein contain effective constituents such as quaternary ammonium salt, glutaraldehyde; Also containing other anti-oxidant (sodium hydrogen phosphate damping fluid), stabilizing agent (triethylene glycol), synergistic agent auxiliary element and cosolvent, solvents etc. such as (ascorbic acid, EDTA), is the complicated preparation system with multiple composition.In real work, how effectively discriminating quaternary ammonium salt (bundleization, strand and two strands) wherein becomes the difficult problem of such quality of the pharmaceutical preparations Control work.
Someone once adopted the method for high performance liquid chromatography UV-detector (HPLC-UV) to differentiate detection; The result finds that the quaternary ammonium salt retention time of bundle and strand is almost consistent; And double-chain quaternary ammonium salt does not have uv absorption, so the HPLC-UV method can't realize the separation discriminating of above-mentioned three types of quaternary ammonium salts.
Wang Yixing etc. (" separating long carbon chain aliphatic amine and quaternary ammonium salt thereof " with thin-layer chromatography; Daily chemical industry; 1989 the 3rd phases: 39-42) with homemade silica G plate; Chloroform in varing proportions (ammoniacal liquor)-methyl alcohol is developping agent, identifies the amine of different carbon chain lengths, and has monitored the synthetic middle partial impurities that generates.The separate object that its operation is directed against is similar amine (as separating single lauryl amine, two lauryl amine and three lauryl amines) and the synthetic pure article (like two octadecyl methyl benzyl ammonium chlorides) that obtain; Different with three types of quaternary ammonium salts in the complicated component sanitizer according to the invention and can't avoid the interference of other compositions in the compound disinfectant, hangover serious; Directly there is obstacle in application, referring to chromatogram 4A.
See to have no a kind of thin-layer chromatography condition can effectively separate above-mentioned three types of quaternary ammonium salts of differentiating in the disinfectant for animals at present from the literature review situation.
Summary of the invention
The invention provides a kind of easy and simple to handle, with low cost, separating effect and significantly separate the method for differentiating bundle, strand and double-chain quaternary ammonium salt in the sanitizer.
For solving the problems of the technologies described above, the present invention takes following technical scheme:
A kind of method of differentiating bundle, strand and double-chain quaternary ammonium salt in the sanitizer of separating may further comprise the steps:
1) chooses bundleization quaternary ammonium salt, strand quaternary ammonium salt and double-chain quaternary ammonium salt standard items respectively and be made into standard solution, simultaneously testing sample is made into concentration solution; The solution solvent for use is a methenyl choloride;
2) draw each solution respectively, put on silica gel g thin-layer plate;
3) the lower floor's solution-methyl alcohol with chloroform and water mixing standing demix is a developping agent, adds in the groove of double flute expansion cylinder, adds strong ammonia solution in another groove, behind the pre-equilibration, launches;
4) take out, dry, put in the iodine vapor smoked after, inspect under the daylight;
5) with whether with the corresponding position of standard items on shown the spot of same color differentiates in the testing sample whether contain these standard items.
The concentration of solution is 0.1mg/mL～1.0mg/mL in the said step 1), preferred 0.5mg/ml; Step 2) the absorption amount is 0.5-1.5 μ l in, is preferably 1 μ l.
The volume ratio of chloroform and water is 20: 1～2 in the step 3), preferred 20: 1.5; The blending ratio of said lower floor solution and methyl alcohol is 10: 2～4 by volume, is preferably 10: 3.
The developping agent addition is 5～15mL in the step 3), preferred 10mL; The addition of strong ammonia solution is 3～5mL, is preferably 4mL.
The pre-equilibration time in the step 3) is 0.5-1.5 hour, is preferably 1 hour.
Exhibition in the step 3) is apart from more than or equal to 10cm, is preferably greater than to equal 13cm.
Said bundle quaternary ammonium salt standard items are for getting benzalkonium chloride C
12, C
14, C
16In the mixing of one or more mass ratioes such as grade; Said double-chain quaternary ammonium salt standard items are two decyl dimethyl bromine ammonium C
10, C
12, C
14, C
16, C
18In the mixing of one or more mass ratioes such as grade; Said strand quaternary ammonium salt standard items are a decyl trimethyl bromine ammonium C
12, C
14, C
18In the mixing of one or more mass ratioes such as grade.
Use the application of said method in the quality control of compound quaternary ammonium salt sanitizer detects also to belong to content of the present invention.
Another purpose of the present invention is to provide a kind of special-purpose developping agent of differentiating in bundleization, strand and the double-chain quaternary ammonium salt method that separates applicable to above-mentioned thin-layer chromatography.
This developping agent is mixed and made into by following two components 10: 2 by volume～4: component one: lower floor's solution is left standstill in 20: 1 by volume～2 the chloroform and the mixing of water; Component two: methyl alcohol.
Two mixture ratios of said developping agent are 10: 3; The blending ratio of said chloroform and water is 20: 1.5.
The invention provides a kind of TLC method of differentiating different classes of (strand, two strands and phenyl ring bundleization) quaternary ammonium salt in the sanitizer that is suitable for separating.Principle of the present invention is to utilize the different classes of quaternary ammonium salt difference of adsorption rate of between silica G adsorbent and developping agent, dissociating, thereby has realized separating and differentiating.The wherein special solvent species of optimizing, developping agent composition, chromatographic condition etc. make the separation that the present invention is directed to three kinds of quaternary ammonium salts and differentiate all very effective.That this method has is easy and simple to handle, with low cost, to advantage such as the instrument and equipment requirement is low; Particularly this method can effectively avoid in quaternary ammonium salt-glutaraldehyde compound preparation other composition to the interference of identification result; Be suitable for popularizing, be applied in the quality control detection to the compound quaternary ammonium salt sanitizer.
Description of drawings
Figure 1A is that the present invention is to the benzalkonium chloride detection limit;
Figure 1B is that the present invention is to first bromine ammonium detection limit in the last of the ten Heavenly stems;
Fig. 2 A is the specificity checking result of the present invention to a decyl trimethyl bromine ammonium of different carbon numbers;
Fig. 2 B is the specificity checking result of the present invention to the didecyl dimethyl bromine ammonium of different carbon numbers;
Fig. 2 C is the specificity checking result of the present invention to the benzalkonium chloride of different carbon numbers;
Fig. 2 D is the specificity checking result (exhibition apart from 10cm) of the present invention to three kinds of different carbon number mixing quaternary ammonium salts;
Fig. 2 E is the specificity checking result (exhibition apart from 13cm) of the present invention to three kinds of different carbon number mixing quaternary ammonium salts;
Fig. 3 A is that the present invention is to compound disinfectant discrimination test result;
Fig. 3 B is that the present invention is to having added the compound disinfectant discrimination test result of strand quaternary ammonium salt;
The result that Fig. 4 A differentiates compound disinfectant for the condition of using in " Wang Yixing " document;
Another groove did not add the result of ammoniacal liquor when Fig. 4 B was pre-equilibration;
Fig. 4 C is for adopting the result of dissolve with methanol sample.
Below in conjunction with specific embodiment the present invention is explained further details.
Embodiment
Embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Method therefor is conventional method if no special instructions among following test and the embodiment.
Instrument and equipment and reagent
Key instrument: AE240 type electronic balance (Switzerland METTLER company); The semi-automatic point sample instrument of Linomat-5 type thin-layer chromatography, Digistore2-digital camera system (Switzerland CAMAG company); Silica gel g thin-layer plate (German MN company).
Main high purity reagent: referring to table 1 (sell because of there being the quaternary ammonium salt reference substance both at home and abroad at present, thus the present invention with following high purity reagent as reference substance, and owing to the part high purity reagent is only done discriminating usefulness, so there is not content value).
Table 1: three types of quaternary ammonium salt reagent
| The reference substance title | Production company | Lot number | Content (%) |
| Benzalkonium chloride C 12 | Fluka?Analytical | 135437943608238 | 99.0 |
| Benzalkonium chloride C 14 | Nanjing optically-active Science and Technology Ltd. | GL1427C20090317 | / |
| Benzalkonium chloride C 16 | Nanjing optically-active Science and Technology Ltd. | GL1627C20090207 | / |
| One decyl trimethyl bromine ammonium C 12 | Fluka?Analytical | 129838211309358 | 99 |
| One decyl trimethyl bromine ammonium C 16 | Nanjing optically-active Science and Technology Ltd. | GL163B20090410 | / |
| One decyl trimethyl bromine ammonium C 18 | Nanjing optically-active Science and Technology Ltd. | GL183C20090310 | / |
| Two decyl dimethyl bromine ammonium C 10 | Tokyo HuaCheng Industry Co., Ltd | K3WTG | / |
| Two decyl dimethyl bromine ammonium C 12 | Nanjing optically-active Science and Technology Ltd. | GL2122B20090404 | / |
| Two decyl dimethyl bromine ammonium C 14 | Tokyo HuaCheng Industry Co., Ltd | FIL01 | 97.0 |
| Two decyl dimethyl bromine ammonium C 16 | Tokyo HuaCheng Industry Co., Ltd | SY04B | 97.0 |
| Two decyl dimethyl bromine ammonium C 18 | Nanjing optically-active Science and Technology Ltd. | GL2182B20090315 | 98.0 |
It is pure that other reagent is analysis.
Differentiate determination experiment
Experimental implementation:
1, formulations prepared from solutions: it is an amount of to get high purity reagent by table 1, adds methenyl choloride respectively and processes the solution that every 1mL all contains 0.5mg table 1 reagent, as reference substance solution.
2, chromatographic condition (TLC method)
1) draws each 1 μ l of above-mentioned solution (0.5-1.5 μ l all can), put on same silica gel g thin-layer plate respectively.
2) earlier chloroform and by volume 20: 1.5 ratio of water are fully mixed, leave standstill, lower floor's solution branch is taken out, be expressed as " chloroform (water) " to layering (because the dissolubility between chloroform and the water is less, so can produce layering).Then; Measure the solution 10ml of lower floor again and add 3ml methyl alcohol (being that blending ratio is by volume 10: 3) as final developping agent, add in the double flute expansion cylinder groove wherein, another groove of double flute expansion cylinder adds the strong ammonia solution of 4mL; Behind the pre-equilibration 1 hour; In the groove that developping agent is arranged, put into a silica gel g thin-layer plate of crossing appearance, launch.
3) take out, dry, put in the iodine vapor smoked after, inspect under the daylight.
3, in the test sample chromatogram, as with the corresponding position of reference substance chromatogram on show the spot of same color, then differentiate to have this contrast quaternary ammonium salt in the test sample.
Below experiment is all accomplished according to above-mentioned experimental implementation, and reagent dosage adds by concrete experimental design.
The selection and the optimization of test one, chromatographic condition
1, the optimization of pre-equilibration condition:
Generally in a groove of double flute expansion cylinder, add developping agent in the prior art, do not add reagent in another groove or add water.In system of the present invention, do not add reagent in another groove or add water, the out-of-flatness of development of chromatogram forward position can appear so that the not parallel irregular problem of spot, referring to Fig. 4 B.Carry out pre-equilibration and in another groove of double flute expansion cylinder, add strong ammonia solution, then preferably resolve the problems referred to above.
The addition of strong ammonia solution can influence the regularity of spot, is the regularity that the strong ammonia solution that adds 4mL under the situation of 13mL can guarantee spot at developping agent, reaches the optimum effect of launching.
Therefore, in order to obtain optimal separating efficiency, the present invention has adopted the method for strong ammonia solution pre-equilibration to solve the irregular and irregular problem in expansion forward position of spot.In the actual detected, the developping agent addition can be 5～15mL, preferred 10mL; The addition of strong ammonia solution is 3～5mL, is preferably 4mL.The pre-equilibration time is 0.5-1.5 hour, is preferably 1 hour.
2, the optimization of developping agent composition:
The developping agent that generally uses in the prior art is chloroform (ammoniacal liquor)-methyl alcohol, is applied in the system of the present invention, and different types of quaternary ammonium salt can't separate and can't avoid in the compound disinfectant other compositions to the interference of identification result.The present invention is through groping, and the developping agent of confirming is chloroform (water)-methyl alcohol.
The usage ratio of chloroform (20mL) and water confirms through experiment, and the result shows, the water yield is in the 1.0mL-2.0mL scope, and along with the increase of the addition of water, benzalkonium chloride is (with benzalkonium chloride C
12Be sample) and the last of the ten Heavenly stems first bromine ammonium (with two decyl dimethyl bromine ammonium C
12Be sample) degree of separation increase gradually, but be increased to 2.0mL above the time when the water yield, the degree of separation of the two increases not obvious even the phenomenon that reduces occurred.Therefore, in the developping agent chloroform and water consumption volume ratio for can be 20: 1～2, optimum 20: 1.5.
Chloroform (water) confirms through experiment that with the consumption of methyl alcohol the result shows, during 10mL chloroform (water); Methanol usage can change in 2～4mL scope; The separating effect that surpasses two kinds of quaternary ammonium salts of this scope is all bad, and chloroform (water) is 10: 2～4 by volume with the blending ratio of methyl alcohol, is preferably 10: 3.
The solvent optimization and the detection limit of test two, sample solution
The present invention has compared the dissolving power and the stability of methyl alcohol and two kinds of solvents of chloroform.The result shows; Though sample and reference substance can both well dissolve in methyl alcohol and methenyl choloride, when being solvent with methyl alcohol, the thin-layer chromatogram repeatability of need testing solution and reference substance solution is very poor; Especially rambling situation often appears in the chromatogram of need testing solution, referring to Fig. 4 C.And when being solvent with the methenyl choloride, the problems referred to above have all obtained good solution, and thin-layer chromatogram repeatability is good, and linear relationship is good.So the present invention is solvent with the methenyl choloride.
Detection limit: take by weighing benzalkonium chloride (C
12) and two last of the ten Heavenly stems first bromine ammonium (C
12) an amount of, add the methenyl choloride dissolving respectively, processing concentration is two types of solution of 0.1mg/ml, 0.5mg/ml, 1.0mg/m, according to above-mentioned chromatographic condition operation.The result shown in Figure 1A (benzalkonium chloride) and Figure 1B (two the last of the ten Heavenly stems first bromine ammonium), wherein, 1:0.1mg/ml; 2:0.5mg/ml; 3:1.0mg/ml.From the color and the depth analysis of spot, this thin-layer chromatography condition to benzalkonium chloride with two last of the ten Heavenly stems first bromine ammonium detection limit all can reach 0.1mg/mL.Therefore, the concentration that detects solution can be 0.1mg/mL～1.0mg/mL, preferred 0.5mg/ml.
Test three, specificity checking
Take by weighing benzalkonium chloride (C
12, C
14, C
16, breviary is B
12, B
14, B
16), two decyl dimethyl bromine ammonium (is called for short first bromine ammonium in the last of the ten Heavenly stems, C
10, C
12, C
14, C
16, C
18, breviary is D
10, D
12, D
14, D
16, D
18), a decyl trimethyl bromine ammonium (C
12, C
14, C
18, breviary is A
12, A
14, A
18) reference substance is an amount of, adds the methenyl choloride dissolving respectively, processes the solution that concentration is 0.5mg/mL, according to above-mentioned chromatographic condition operation.Result such as Fig. 2 A (0.5mg/mL one decyl trimethyl bromine ammonium, 1A
12, 2A
14, 3A
18) and Fig. 2 B (the two decyl dimethyl bromine ammoniums of 0.5mg/mL, 1D
10, 2D
12, 3D
14, 4D
16, 5D
18) and Fig. 2 C (0.5mg/mL benzalkonium chloride, 1B
12, 2B
14, 3B
16), show that similar quaternary ammonium salt exhibition is apart from identical.
It is an amount of that other gets above-mentioned reference substance, adds methenyl choloride and make dissolving, and the quaternary ammonium salt of similar different carbon numbers is processed three parts of mixed solutions that concentration all is about 0.5mg/mL, i.e. benzalkonium chloride mixed solution (B respectively by the mixing of quality geometric ratio
Mix), two decyl dimethyl bromine ammonium mixed solution (D
Mix), a decyl trimethyl bromine ammonium mixed solution (A
Mix), according to above-mentioned chromatographic condition operation.(exhibition is apart from equaling 10cm, 1:D for result such as Fig. 2 D
Mix, 2:A
Mix, 3:B
Mix) and Fig. 2 E (exhibition is apart from equaling 13cm, 1:A
Mix, 2:B
Mix, 3:D
Mix) shown in, Fig. 2 D is different with the mixed solution Rf value of three kinds of quaternary ammonium salts among Fig. 2 E, and spot is distributed in different height, therefore can effectively distinguish discriminating, proves that the discriminating that the present invention is directed to three types of quaternary ammonium salts has good specificity.
On the other hand, Fig. 2 D shows that the Rf value of similar quaternary ammonium salt is identical, shows as same spot on the chromatogram when the exhibition distance equals 10cm; Fig. 2 E shows that two decyl dimethyl bromine ammonium class quaternary ammonium salts (are D when opening up distance greater than 13cm
10, D
12, D
14, D
16, D
18) difference appears in each other Rf value, shows as a string spot on the chromatogram, this just shows suitable raising exhibition distance, helps to separate to differentiate similar quaternary ammonium salt, further the proof discriminating that the present invention is directed to three types of quaternary ammonium salts has good specificity.Therefore exhibition is apart from more than or equal to 10cm when confirming to detect, and is preferably greater than to equal 13cm.
Test four, TLCP serviceability test
The present invention has also compared silica G, GF254 and H plate.As a result, after adopting identical developping agent to launch, no any spot appears on GF254 plate and the H plate, shows that GF254 plate and H plate discomfort are fit to do such discriminating.And the G plate presents spot after iodine vapor is smoked, so the present invention selects the G plate for use.
Sample: compound quaternary ammonium salt-glutaraldehyde disinfectant and two kinds of reference substances
Method:
1, formulations prepared from solutions: get disinfectant for animals sample 1mL, place separating funnel, add methenyl choloride 10mL, shake well is obtained the solution 1mL of lower floor and is placed the scale test tube, adds methenyl choloride to 5mL, as need testing solution.Other gets benzalkonium chloride (C
12) and two last of the ten Heavenly stems first bromine ammonium (C
12) high purity reagent is an amount of, add methenyl choloride respectively and process the solution that every 1mL contains 0.5mg, as reference substance solution.
2, chromatographic condition (TLC method)
1) draws each 1 μ L of above-mentioned solution, put on same silica gel g thin-layer plate respectively.
2) be that (chloroform (water): methyl alcohol=10: 3) in the double flute expansion cylinder, add the 13mL developping agent in the groove, add the strong ammonia solution of 4mL in another groove, pre-equilibration launched after 1 hour developping agent with 20: 1.5 chloroform (water) lower floor solution-methyl alcohol.
3) take out, dry, put in the iodine vapor smoked after, inspect under the daylight.
3, result: result such as Fig. 3 A (1, benzalkonium chloride (C
12); 2, need testing solution; 3, the last of the ten Heavenly stems first bromine ammonium (C
12)) shown in, visible test sample with the corresponding position of reference substance chromatogram on shown and the spot of same color shown that this method can effectively identify the benzalkonium chloride (C that contains in the sample
12) and two last of the ten Heavenly stems first bromine ammonium (C
12) two kinds of quaternary ammonium salts.
Sample: added a decyl trimethyl bromine ammonium (C
12) compound quaternary ammonium salt-glutaraldehyde disinfectant and three kinds of reference substances
Method:
1, formulations prepared from solutions: get disinfectant for animals sample 1mL and 25mg one decyl trimethyl bromine ammonium (C
12) high purity reagent, place separating funnel, add methenyl choloride 10mL, shake well is obtained the solution 1mL of lower floor and is placed the scale test tube, adds methenyl choloride to 5mL, as need testing solution.Other gets a decyl trimethyl bromine ammonium (C
12), benzalkonium chloride (C
12), two last of the ten Heavenly stems first bromine ammonium (C
12) high purity reagent is an amount of, add methenyl choloride respectively and process the solution that every 1mL contains 0.5mg, as reference substance solution.
2, chromatographic condition (TLC method)
1) draws each 1 μ L of above-mentioned solution, put on same silica gel g thin-layer plate respectively.
2) be that (chloroform (water): methyl alcohol=10: 3) in the double flute expansion cylinder, add the 13mL developping agent in the groove, add the strong ammonia solution of 4mL in another groove, pre-equilibration launched after 1 hour developping agent with 20: 1.5 chloroform (water) lower floor solution-methyl alcohol.
3) take out, dry, put in the iodine vapor smoked after, inspect under the daylight.
3, result: result such as Fig. 3 B (1, one decyl trimethyl bromine ammonium (C
12); 2, need testing solution; 3, benzalkonium chloride (C
12); 4, the last of the ten Heavenly stems first bromine ammonium (C
12)) shown in, visible test sample with the corresponding position of reference substance chromatogram on shown and the spot of same color shown that this method can effectively identify a decyl trimethyl bromine ammonium (C who contains in the sample
12), benzalkonium chloride (C
12) and two last of the ten Heavenly stems first bromine ammonium (C
12) three kinds of quaternary ammonium salts.
Claims (13)
1. one kind is separated the method for differentiating bundle, strand and double-chain quaternary ammonium salt in the sanitizer, may further comprise the steps:
1) chooses bundleization quaternary ammonium salt, strand quaternary ammonium salt and double-chain quaternary ammonium salt standard items respectively and be made into standard solution, simultaneously testing sample is made into concentration solution; The solution solvent for use is a methenyl choloride;
2) draw each solution respectively, put on silica gel g thin-layer plate;
3) the lower floor's solution-methyl alcohol with chloroform and water mixing standing demix is a developping agent, adds in the groove of double flute expansion cylinder, adds strong ammonia solution in another groove, behind the pre-equilibration, launches;
4) take out, dry, put in the iodine vapor smoked after, inspect under the daylight;
5) with whether with the corresponding position of standard items on shown the spot of same color differentiates in the testing sample whether contain these standard items.
2. according to the method for the said separation discriminating of claim 1 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the concentration of solution is 0.1mg/mL～1.0mg/mL in the said step 1); Step 2) the absorption amount is 0.5-1.5 μ l in.
3. according to the method for the said separation discriminating of claim 2 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the concentration of solution is 0.5mg/ml in the said step 1); Said step 2) the absorption amount is 1 μ l in.
4. according to the method for the said separation discriminating of claim 1 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the volume ratio of chloroform and water is 20: 1～2 in the said step 3); The blending ratio of said lower floor solution and methyl alcohol by volume is 10: 2～4.
5. according to the method for the said separation discriminating of claim 4 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the volume ratio of chloroform and water is 20: 1.5 in the said step 3); The blending ratio of said lower floor solution and methyl alcohol by volume is 10: 3.
6. according to the method for the said separation discriminating of claim 1 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the developping agent addition is 5～15mL in the said step 3); The addition of strong ammonia solution is 3～5mL.
7. according to the method for the said separation discriminating of claim 6 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the developping agent addition is 10mL in the said step 3); The addition of strong ammonia solution is 4mL.
8. according to the method for the said separation discriminating of claim 1 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the pre-equilibration time in the said step 3) is 0.5-1.5 hour.
9. the method for bundleization, strand and double-chain quaternary ammonium salt is differentiated in said according to Claim 8 separation, and it is characterized in that: the pre-equilibration time in the said step 3) is 1 hour.
10. according to the method for the said separation discriminating of claim 1 bundleization, strand and double-chain quaternary ammonium salt, it is characterized in that: the exhibition distance in the said step 3) is more than or equal to 10cm.
11. the method for bundleization, strand and double-chain quaternary ammonium salt is differentiated in said separation according to claim 10, it is characterized in that: the exhibition distance in the said step 3) is more than or equal to 13cm.
12. the method for bundleization, strand and double-chain quaternary ammonium salt is differentiated in each said separation according to claim 1-11, it is characterized in that: said bundle quaternary ammonium salt standard items are for getting benzalkonium chloride C
12, C
14, C
16In the mixing of one or more mass ratioes such as grade; Said double-chain quaternary ammonium salt standard items are two decyl dimethyl bromine ammonium C
10, C
12, C
14, C
16, C
18In the mixing of one or more mass ratioes such as grade; Said strand quaternary ammonium salt standard items are a decyl trimethyl bromine ammonium C
12, C
14, C
18In the mixing of one or more mass ratioes such as grade.
13. the application of each said method of claim 1-11 in the quality control of compound quaternary ammonium salt sanitizer detects.
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| CN103323539A (en) * | 2012-11-28 | 2013-09-25 | 泰州市产品质量监督检验所 | High performance liquid chromatography method for determination of benzalkonium chloride content in antiseptic wipes |
| CN103245738B (en) * | 2013-04-18 | 2014-09-10 | 北京民海生物科技有限公司 | Measuring method of CTAB content in meningococcal polysaccharide |
| CN109406698B (en) * | 2018-11-30 | 2020-12-25 | 广州中科检测技术服务有限公司 | Method for measuring content of single-chain substituted dimethyl benzyl ammonium chloride by HPLC |
| CN111751189A (en) * | 2020-07-27 | 2020-10-09 | 广东石油化工学院 | Method for determining quaternary ammonium salt disinfectant residue of dairy product based on QuEChERS purification technology |
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