Tetrabutylammonium hydrogen sulfate (TBAHS) can be used as surfactant, catalyst, emulsifier, disinfectant, bactericide, antistatic agent, etc. Tetrabutylammonium bisulfate buffer salt system is often used as aqueous mobile phase in reversed-phase liquid chromatography detection, and can often produce excellent separation effects for some compound pairs with special structures and difficult to separate. Its application examples are as follows:
1) Taking moxifloxacin hydrochloride injection as an example, the main related substances include: N-methyl impurity, impurity A, impurity B, impurity C, impurity D, and impurity E. The analytical method of the related substance that Chinese Pharmacopoeia, European Pharmacopoeia and American Pharmacopoeia provide is reversed-phase liquid chromatography, is filler with phenyl bonded silica gel, and mobile phase is acetonitrile-salt solution (get tetrabutylammonium bisulfate 0.5g, Potassium dihydrogen phosphate 1g, add water 500mL, add phosphoric acid 2mL, dilute with water to 1000mL) (volume ratio 30:70), detection wavelength is 293nm, flow rate is 1.3mL/min, column temperature is 30°C, injection volume is 20μL. The mobile phase can effectively separate moxifloxacin and its impurities.
2) Used in the detection of carboplatin content and related substances in carboplatin and carboplatin injection, using high performance liquid chromatography, using octadecylsilane bonded silica gel column, and using mobile phase A and mobile phase B Gradient elution, the flow rate is 0.4-0.6mL/min, the column temperature is 25-30°C, and the detection wavelength is 220nm; the mobile phase A is tetrabutylammonium bisulfate buffer, 20mL is diluted with water to 1000mL; The mobile phase B is tetrabutylammonium hydrogensulfate buffer, get 20mL and add water to dilute to 750mL, add acetonitrile 240-260mL; described tetrabutylammonium hydrogensulfate buffer is 8.5g tetrabutylammonium hydrogensulfate, Add 80mL of water to dissolve, then add 3.4mL of phosphoric acid, and finally adjust the pH value to 7.3-7.7 with 10mol/mL sodium hydroxide solution; the gradient elution is carried out with mobile phase A and mobile phase B, time (min)/flow Phase B (v%): 0/0; 10/0; 35/100; 40/100; 41/0; 55/0. Compared with the prior art, the above detection method obviously improves the retention performance, and has the characteristics of strong specificity, high sensitivity and good accuracy.
3) It is used for the determination of ammonium acetoacetamide sulfamate in the production of acesulfame-K, the main steps are: (1) Select the analytical chromatographic conditions: ODS column (4.6mm×25cm) or other equivalent chromatographic columns, wavelength 250nm, flow rate 1ml/min, column temperature 25°C, injection volume 20ul; (2) Prepare tetrabutylammonium hydrogensulfate solution with deionized water to a molar concentration of 1.0~2.0mmol/L, and prepare tetrabutylammonium hydrogensulfate solution and chromatographic grade methanol in a volume ratio of 60:40 to make a mobile phase; (3) dilute the sample to be tested with an organic solvent to a concentration of 0.5% to 2.0% by volume to prepare a test solution; (4) use a trace Syringe draws test solution, injects high performance liquid chromatograph, analyzes with area external standard method; (5) record the content of ammonium acetoacetylsulfame in the sample to be measured. The method can accurately and quickly determine the content of ammonium acetoacetamide sulfamate.
4) Catalysts for the synthesis of benzyl alkyl disulfide, using thiourea and benzyl thiocyanide as sulfur sources, alkyl halides as raw materials, potassium iodide and tetrabutylammonium bisulfate as catalysts, potassium phosphate as base, Reaction in water to obtain unsymmetrical benzyl alkyl disulfide compounds. The method of the present invention avoids the use of mercaptan with pungent smell as a sulfur source, and adopts microwave reaction technology and "one pot method", which not only can achieve the purpose of environmental protection, but also simplifies the operation procedure and further reduces the synthesis and scale cost of production.
5) It is used to prepare a trivalent chromium electroplating solution, which is composed of the following raw material components: 10-15 parts of hydroxychromium sulfate, 8-10 parts of chromium trichloride, 5-8 parts of cobalt nitrate, 3-5 parts Aluminum sulfate, 3-5 parts of potassium carbonate, 5-8 parts of potassium nitrate, 3-5 parts of ammonium chloride, 2-3 parts of octadecyl dimethyl benzyl ammonium chloride, 1-2 parts of tetrabutyl Ammonium bromide, 2-3 parts of tetrabutylammonium bisulfate, 8-10 parts of hydrochloric acid, 5-8 parts of oxalic acid, 1-3 parts of sodium pyrophosphate, 2-3 parts of disodium dihydrogen pyrophosphate, 2-3 parts Glycine, 3-4 parts of aminocaproic acid, 80-100 parts of deionized water.
The trivalent chromium electroplating solution only precipitates oxygen during the chromium plating process, is clean and pollution-free, has a bright appearance, few cracks, good bonding force, rich source of raw materials, low cost, excellent cost performance, and good stability of the electroplating solution. for its industrialization.
Tetrabutyl quaternary ammonium salt is a phase transfer catalyst with superior performance. Tetrabutylammonium bisulfate buffer salt system is commonly used as aqueous mobile phase in reversed-phase liquid chromatography detection, but, with the raising of tetrabutylammonium bisulfate concentration, the stability of tetrabutylammonium bisulfate buffer salt system Gradually decreases. Tetrabutylammonium bisulfate buffered saline solution must be prepared immediately before use, and the use time should not exceed 6 hours (obvious turbidity can be seen after 8 hours at room temperature), otherwise it will cause chromatographic peak drift or even salt in the pump or column Precipitation leading to pump and column damage.
The production process of tetrabutylammonium bisulfate includes the drying process, because tetrabutylammonium bisulfate is highly water-soluble, and it is necessary to ensure that the storage environment is dry, cool and away from compatible substances during storage. Before drying, it must be guaranteed to be dry without water, so the drying process has a great influence on the quality of tetrabutylammonium bisulfate.
The drying of tetrabutylammonium bisulfate is usually carried out in a dryer, and most of the dryers are double-cone-shaped drying cylinders. In order to prevent tetrabutylammonium bisulfate from contacting with the external environment and causing pollution, the drying cylinder is usually set to be sealed. The water vapor evaporated from the solid during the drying process cannot be discharged in time, and the high-temperature water vapor accumulates in the cylinder, which not only affects the drying effect, but also easily causes safety accidents if the pressure in the cylinder is too high.