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Liquid phase chromatography analysis method for active ingredient content of crude product M

A technology of liquid chromatography analysis and high performance liquid chromatography, which is applied in the direction of analyzing materials, measuring devices, and material separation, and can solve problems such as unclear reaction mechanisms

Inactive Publication Date: 2012-03-14
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the aniline process is very mature, its reaction mechanism is not yet clear

Method used

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  • Liquid phase chromatography analysis method for active ingredient content of crude product M
  • Liquid phase chromatography analysis method for active ingredient content of crude product M
  • Liquid phase chromatography analysis method for active ingredient content of crude product M

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0010] Use a high-angle weighing bottle to weigh 25 mg of MBT sample, add 10 ml of methanol solution to it, put it in an ultrasonic cleaner and vibrate for 5 minutes, take it out and transfer it to a 250 ml volumetric flask, dilute to the mark with methanol, shake well, and filter to configure 0.1 mg / mL solution; the column temperature is kept at 20°C, the liquid chromatography is a VWD detector, the column model is EXTEND-C18, the liquid chromatography uses water and methanol as the mobile phase, the flow rate is 1ml / min, and the wavelength of the VWD detector is 254nm , use a micro injector to inject 5 μl of sample into the liquid chromatography, and the gradient program is: when the injection time is 0 minutes, the proportion of water in the mobile phase is 90%, and the proportion of methanol is 10%; The proportion of water in the middle is 30%, and the proportion of methanol is 70%; in 22 minutes, the proportion of water in the mobile phase is 0%, and the proportion of meth...

example 2

[0015] Weigh 50 mg of MBT sample with a high-angle weighing bottle, add chromatographically pure methanol solution into it, put it in an ultrasonic cleaner and vibrate for 10 minutes, take it out and transfer it to a 250ml volumetric flask, dilute to the mark with methanol, shake well, and filter to configure 0.2mg / mL solution; keep the room temperature at 23°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 1ml / min, the wavelength of the VWD detector is 254nm, inject 5μl of sample into the liquid chromatography with a micro injector, the gradient The program is: when the injection time is 0 minutes, the proportion of water in the mobile phase is 90%, and the proportion of methanol is 10%; at 15 minutes, the proportion of water in the mobile phase is 30%, and the proportion of methanol is 70%; 22 At 30 minutes, the proportion of water in the mobile phase was 90%, and the proportion of methanol was 10%. Parallel samples were performed 5 ti...

example 3

[0017] Use a high-angle weighing bottle to weigh 125 mg of MBT sample, add 100 ml of methanol solution to it, put it in an ultrasonic cleaner and vibrate for 20 minutes, take it out and transfer it to a 250 ml volumetric flask, dilute to the mark with methanol, shake well, and filter to configure 0.5 mg / mL solution; keep the room temperature at 27°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 1.0ml / min, and the wavelength of VWD detector is 254nm. The program is: when the injection time is 0 minutes, the proportion of water in the mobile phase is 900%, and the proportion of methanol is 10%; at 15 minutes, the proportion of water in the mobile phase is 30%, and the proportion of methanol is 70%; 22 At 30 minutes, the proportion of water in the mobile phase was 90%, and the proportion of methanol was 10%. Parallel samples were performed 5 times with good repeatability. The above effective substances are quantified, and their purity is ...

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Abstract

The invention relates to a liquid phase chromatography analysis method for the active ingredient content of a crude product M. The method comprises the following steps of: weighing crude MBT (2-Mercaptobenzothiazole) with a weighing bottle, preparing a 0.1-0.5 mg / mL sample with a chromatographically pure methanol solution, and putting the sample into an ultrasonic cleaner for oscillating for 2-20 minutes; filtering the sample solution with 0.2 mum of filtering film before sampling; keeping the column temperature at 20-30 DEG C, wherein a liquid phase chromatogram is a VWD (Variable Wavelength Detector), the model of the chromatogram column is EXETEND-C18, and water and methanol are taken as a flowing phase of the liquid phase chromatogram; and injecting 5 mu l of sample into liquid phase chromatogram with a trace sampler, wherein the gradient process is that: when the sampling time is 0 minute, the ratio of water in the flowing phase is 90 percent while the ratio of methanol is 10 percent; when the sampling time is 15 minutes, the ratio of the water in the flowing phase is gradually decreased to 30 percent while the ratio of the methanol is 70 percent; when the sampling time is 22 minutes, the ratio of the water in the flowing phase is 0 percent while the ratio of the methanol is 100 percent; and when sampling time is 30 minutes, the ratio of the water in the flowing phase is increased gradually to 90 percent while the ratio of the methanol is 10 percent. Under the analyzing condition, each active ingredient can be effectively separated.

Description

technical field [0001] The invention relates to a liquid chromatography analysis method for the effective component content of crude rubber vulcanization accelerator 2-mercaptobenzothiazole (MBT), belonging to the technical field of rubber vulcanization accelerator MBT analysis. Background technique [0002] Accelerator M is a general-purpose rubber vulcanization accelerator, and it is also the parent material of most sulfenamide accelerators. The synthesis of accelerators such as benzothiazole zinc salt, sulfenimide, sulfenamide, etc., cannot be separated from the development of accelerator M. The quality and output of accelerator M are directly related to the development of the rubber industry. At present, the high-pressure aniline method is widely used in China for production. That is, aniline, carbon disulfide, and sulfur are reacted under high temperature and high pressure to form a crude product, and then refined to obtain a finished product. The source of raw materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 安静
Owner KEMAI CHEM
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