CN102393424A - Analytic method for purity of N-cyclohexyl-2-benzothiazole sulfonamide as thiofide

Info

Abstract

Description

Claims

CN102393424A

Publication number: CN102393424A
Application number: CN2011102475872A
Authority: CN
Inventors: 马淑伟
Original assignee: Kemai Chemical Co Ltd
Current assignee: Kemai Chemical Co Ltd
Priority date: 2011-08-24
Filing date: 2011-08-24
Publication date: 2012-03-28

The invention relates an analytic method for the purity of N-cyclohexyl-2-benzothiazole sulfonamide as thiofide and discloses a liquid chromatogram analytic method for the purity of thiofide CBS. The method comprises the following steps of: accurately weighing a proper amount of standard sample; preparing a standard sample solution; accurately weighing a proper amount of test sample; preparing a test sampling solution with the same concentration, wherein two solutions use C18 columns; and carrying out discrimination and purity measurement on the solution by adopting an ultraviolet or diode array detector under the detection conditions that the column temperature is 20-30DEG C, a mobile phase is a mixed solution (volume ratio) of 5-100 percent of methanol and 95 percent of water, the flow speed of the mobile phase is 0.5-5.0ml/min and the detection wavelength is 100-400nm.

The analytical approach of thiofide N cyclohexyl 2 benzothiazole sulfenamide purity

Technical field

The present invention relates to the liquid phase chromatography analytical method of a kind of thiofide N cyclohexyl 2 benzothiazole sulfenamide (CBS) purity, the quality control of CBS is had good action, its technical field belongs to the thiofide analytical approach.

Background technology

Along with the development of rubber industry, the research of vulcanization accelerator more and more receives people's attention with production.Vulcanization accelerator plays important effect in vulcanization of rubber process; It can be accelerated the reaction of rubber and vulcanizing agent greatly and boost productivity; Also can improve simultaneously the physical and mechanical properties of vulcanized rubber, CBS is the requisite a kind of primary accelerator of present rubber industry.The purity of vulcanization accelerator CBS has very big influence to the quality of downstream product, and therefore, the purity of measuring CBS accurately has decisive meaning for the production of downstream product.At present, the analytical approach of CBS purity is mainly acid base titration, and the alkaline matter of non-CBS also has contribution to titration results in the sample, causes the purity titration results of CBS bigger than normal than actual value.Along with the progress of analytical technology and chromatographic popularizing, existing its purity is adopted high performance liquid chromatography, this method has precision height, accuracy is high, highly sensitive, specificity is strong advantage.

The molecular structure of CBS is following:

Summary of the invention

The invention provides a kind of liquid phase chromatography analytical method of rubber vulcanizing accelerator CBS purity, this method show as with a kind of efficient liquid-phase chromatography method can science, effectively, easily it is carried out quality control.

Technical scheme of the present invention is:

The preparation of 1 testing sample solution (being used for differentiating and purity testing)

Precision takes by weighing testing sample, also dilutes the solution of processing 0.01～2mg/ml with dissolution with solvents, as testing sample solution.

The preparation of 2 standard solutions (being used for differentiating and purity testing)

Precision takes by weighing standard items, processes the solution with isoconcentration with homogeneous solvent dissolving and dilution, as standard solution.

3 measure

Step 1,2 solution are used same C18 post sample introduction respectively; 20～30 ℃ of column temperatures, moving phase is the mixed liquor of first alcohol and water, and volume ratio is a methyl alcohol 60～100%; Water 0～40%; Flow rate of mobile phase is 1.0～1.5ml/min, and detecting wavelength is under the testing conditions of 254～350nm, adopts ultraviolet or PDAD that it is differentiated and purity testing.

Described solvent is ethanol, methenyl choloride or tetrahydrofuran

Described C18 post is preferably XDB-C185um 4.6*250mm.Described flow rate of mobile phase is preferably 1.5ml/min.Described detection wavelength is preferably 280nm.

Liquid phase analysis method of the present invention can carry out the discriminated union detection by quantitative to CBS, and purity precision is ± 0.2%.

Description of drawings

Fig. 1 is that embodiment 1 methyl alcohol changes synoptic diagram in time;

Fig. 2 is that embodiment 2 methyl alcohol change synoptic diagram in time;

Fig. 3 is that embodiment 3 methyl alcohol change synoptic diagram in time.

Embodiment

Embodiment 1:

Take by weighing CBS sample 1mg with the measuring cup precision,, be put in the ultrasonic cleaner and vibrated 5 minutes, transfer to after the taking-up in the volumetric flask of 100ml, be diluted with ethanol to scale, shake up to wherein adding 5ml ethanol reagent; 30 ℃ of column temperatures, flow velocity are 1.0ml/min, and the UV-detector wavelength is 254nm, SB-C185um 4.6*250mm, and to liquid chromatography injected sample 10 μ l, eluent gradient is following with microsyringe:

It is as shown in Figure 1 that methyl alcohol changes synoptic diagram in time;

Consistent according to standard solution with the retention time of the main peak of testing sample solution, be judged to be CBS,

By the purity of external standard method with the long-pending calculating in main composition sharp side testing sample.

?	Standard items	Instance 1
			Main peak retention time (min)	22.538	22.549
Purity (%)	99.50	97.72

Main composition peak theoretical cam curve: N=60173.

Embodiment 2:

Take by weighing CBS sample 50mg with the measuring cup precision,, be put in the ultrasonic cleaner and vibrated 5 minutes, transfer to after the taking-up in the volumetric flask of 100ml, be diluted to scale, shake up, get an amount of filtration with tetrahydrofuran to wherein adding 10ml tetrahydrofuran reagent; 25 ℃ of column temperatures, flow velocity are 1.5ml/min, and the UV-detector wavelength is 280nm, and chromatographic column is XDB-C185um 4.6*250mm, and to liquid chromatography injected sample 10 μ l, eluent gradient is following with microsyringe:

It is as shown in Figure 2 that methyl alcohol changes synoptic diagram in time;

Example 1 is differentiated with purity and is calculated together.

?	Standard items	Instance 2
			Main peak retention time (min)	15.712	15.757
Purity (%)	99.50	97.73

Main composition peak theoretical cam curve: N=65982

Embodiment 3:

Take by weighing CBS sample 200mg with the measuring cup precision,, be put in the ultrasonic cleaner and vibrated 5 minutes, transfer to after the taking-up in the volumetric flask of 100ml, be diluted to scale, shake up, get an amount of filtration with methenyl choloride to wherein adding 20ml methenyl choloride reagent; 20 ℃ of column temperatures, flow velocity are 1.5ml/min, and the UV-detector wavelength is 350nm, RX-C185um 4.6*250mm, and to liquid chromatography injected sample 10 μ l, eluent gradient is following with microsyringe:

It is as shown in Figure 3 that methyl alcohol changes synoptic diagram in time;

Example 1 is differentiated with purity and is calculated together.

?	Standard items	Instance 3
			Main peak retention time (min)	14.369	14.373
Purity (%)	99.50	97.75

Main composition peak theoretical cam curve: N=58998

Same lot sample article are done two parallel appearance with chemical titration, record sample purity and are respectively: 98.47% and 97.93%, and mean value is: 98.20%

Time (min)

Methyl alcohol

1. the analytical approach of thiofide N cyclohexyl 2 benzothiazole sulfenamide purity is characterized in that adopting liquid phase chromatography analytical method.

2. the method for claim 1 is characterized in that method step is following:

1) preparation of testing sample solution: accurately take by weighing testing sample, also dilute the solution of processing 0.01～2mg/ml with dissolution with solvents, as testing sample solution;

2) preparation of standard solution: accurately take by weighing standard items, process solution with homogeneous solvent dissolving and dilution, as standard solution with isoconcentration;

3) solution mensuration: with step 1), 2) uses the C18 post; 20～30 ℃ of column temperatures, moving phase is the mixed liquor of first alcohol and water, and volume ratio is a methyl alcohol 60～100%; Water 0～40%; Flow rate of mobile phase is 1.0～1.5ml/min, and detecting wavelength is under the testing conditions of 254～350nm, adopts ultraviolet or PDAD that it is differentiated and purity testing.

3. method as claimed in claim 2 is characterized in that described solvent is ethanol, methenyl choloride or tetrahydrofuran.

4. method as claimed in claim 2 is characterized in that described C18 post, is preferably XDB-C18 5um4.6*250mm.

5. method as claimed in claim 2 is characterized in that described flow rate of mobile phase is preferably 1.5ml/min.

6. method as claimed in claim 2 is characterized in that described detection wavelength is preferably 280nm.