CN111735884A

CN111735884A - High performance gas chromatography detection method for triethylamine content in feed liquid

Info

Publication number: CN111735884A
Application number: CN202010773654.3A
Authority: CN
Inventors: 刘利聪; 李斌水; 马静; 何连顺; 张玉锋; 冯立双; 王阳
Original assignee: Jing Jing Pharmaceutical Co ltd
Current assignee: Jing Jing Pharmaceutical Co ltd
Priority date: 2020-08-04
Filing date: 2020-08-04
Publication date: 2020-10-02

Abstract

The invention discloses a high-efficiency gas chromatography detection method for triethylamine content in feed liquid, and belongs to the technical field of column chromatography. (1) Determining chromatographic conditions (2), balancing an instrument system and preparing a chromatographic column (3) reference solution by using a triethylamine sample solution headspace sample injection 10 needles: preparing a reference substance solution with the concentration of 2mg/ml by using sodium hydroxide, adding the reference substance solution into a headspace bottle containing 0.6 gAR-grade sodium chloride, capping, and ultrasonically dissolving (4) a test substance solution: adding 1ml of 1mol/L sodium hydroxide solution into 1ml of a test sample, placing the test sample into a headspace bottle containing 0.6g of sodium chloride AR, pressing a cover, ultrasonically dissolving (5) triethylamine sample solution, reference substance solution and test sample solution in a valve box for balancing 30min for sample injection, recording peak areas, and calculating results according to an external standard method. The method can well separate the triethylamine in the feed liquid from other component peaks, and is suitable for measuring the triethylamine content of various complex components.

Description

High performance gas chromatography detection method for triethylamine content in feed liquid

Technical Field

The invention belongs to the technical field of column chromatography, and particularly relates to a high-efficiency gas chromatography detection method of triethylamine.

Background

Triethylamine can be used as solvent, catalyst and raw material in organic synthesis. Can be used for preparing catalyst of phosgene method polycarbonate, polymerization inhibitor of tetrafluoroethylene, rubber vulcanization accelerator, special solvent in paint remover, enamel anti-hardening agent, acid-binding agent, surfactant, preservative, bactericide, ion exchange resin, dye, spice, medicine, high-energy fuel, liquid rocket propellant and the like. Among the products that consume triethylamine in the pharmaceutical field are: ampicillin sodium, amoxicillin, pioneer IV, cefazolin sodium, piperazine penicillin, ketoconazole, vitamin B6, penicillamine berberine hydrochloride and alprazolam, o-chlorophenylacetic acid and pipemidic acid.

Triethylamine has inhalation toxicity, and can cause pulmonary congestion, hemorrhage, peribronchitis, myocardial degeneration, liver and kidney congestion, degeneration and necrosis; reproductive toxicity has an effect on development; flammable, the vapor of which mixes with air to form an explosive mixture. It can cause combustion and explosion when meeting high heat and open fire. Can react with oxidant strongly. Its vapor is heavier than air and can diffuse to a considerable distance at a lower position, causing a flashback in the case of an open flame. Has corrosive property.

Triethylamine is one of the raw materials for producing pantoic acid, and the content and the residual amount thereof need to be detected because of the toxicity. In the existing triethylamine gas phase detection method in the literature, linear unqualified (R2 is less than 0.9) occurs in practical verification, and the repeatability is poor, so that larger errors are caused, and the deviation of experimental data is larger. And the acid-base titration detection method of triethylamine is only suitable for content determination of triethylamine samples with single components, and accurate results cannot be determined by the acid-base titration method due to the influence of the components such as triethylamine, strong base, isobutyraldehyde and the like contained in feed liquid. The method adopted by the invention has high accuracy and small error, and can effectively detect experimental and production data.

Disclosure of Invention

Aiming at the technical problems in the prior art, the invention aims to provide a high-efficiency gas chromatography detection method for triethylamine content in feed liquid, which can well separate the triethylamine in the feed liquid from other component peaks and is suitable for the determination of the triethylamine content of various complex components.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a high-efficiency gas chromatography detection method of triethylamine content in feed liquid,

the chromatographic conditions were as follows:

a chromatographic column: amine gas chromatographic column

Column temperature: 50 ℃; sample inlet temperature: 240 ℃; detector temperature: 280 ℃;

sample bottle: 80 ℃; a valve box: 90 ℃; pipeline: 100 ℃;

the method comprises the following steps:

(1) setting a high performance gas chromatograph according to chromatographic conditions;

(2) balancing an instrument system and a chromatographic column by using 10 needles of triethylamine sample solution with the concentration of 50% in headspace sample injection; preparation of a sample solution: adding 1ml triethylamine sample and 1ml 1mol/L sodium hydroxide solution into a headspace bottle containing 0.6 gAR-grade sodium chloride, and pressing a cover to perform ultrasonic dissolution;

(3) preparing a reference substance solution: precisely weighing a triethylamine reference substance into a 50ml volumetric flask, dissolving with 1mol/L sodium hydroxide solution for constant volume, after dilution, precisely weighing 2ml, adding into a headspace flask containing 0.6 gAR-grade sodium chloride, capping, ultrasonically dissolving, and performing high performance gas chromatography analysis under the chromatographic conditions to obtain a standard curve chart and a linear equation;

(4) preparing a test solution: precisely measuring 1ml of a sample, adding 1ml of 1mol/L sodium hydroxide solution, placing into a headspace bottle containing 0.6g of sodium chloride AR, capping, and ultrasonically dissolving;

(5) and (4) carrying out high performance gas chromatography analysis on the test solution, recording the peak area, and calculating the result according to an external standard method.

In step (1), the sample injection is required to be carried out within 3 hours.

The chromatographic column is Agilent CP-Volamine.

And (3) balancing the triethylamine sample solution, the reference substance solution and the test sample solution in a valve box for 30min, and then injecting samples.

Triethylamine is active in property, the sample feeding process is not easy to balance after the triethylamine is dissolved in water, the repeatability of a detection result is poor, 1mol/L sodium hydroxide is used as a solvent, the triethylamine can be replaced by strong base, and sodium chloride is added to enable the solution in a headspace bottle to reach a saturated state, so that the triethylamine is balanced in the sample feeding process, and a more accurate detection result is obtained.

Drawings

FIG. 1 is a standard curve diagram of linear relation of triethylamine

FIG. 2 is a chromatogram of a sample in an example of the present invention

The invention has the beneficial effects that:

the method has the advantages of convenient and quick detection process, high accuracy of detection results and good consistency; sodium hydroxide is selected as a solvent, and sodium chloride is added, so that the detection amount of triethylamine is increased, peaks of triethylamine and other components in the feed liquid can be well separated, and the method is suitable for determination of triethylamine content of various complex components.

Detailed Description

The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.

In the following examples, the high performance gas chromatograph used was shanghai shen fen GC 9600; the chromatographic column is Agilent CP-Volamine 30m x 0.32 mm; the headspace sample injector is DK-3001A; the invention can also adopt high-efficiency gas chromatographs of other manufacturers and models, amine chromatographic columns of other models and lengths and other sample introduction concentrations to achieve the aim of the invention.

Examples

Chromatographic conditions are as follows:

a chromatographic column: agilent CP-Volamine

Column temperature: 50 ℃, injection port temperature: 240 ℃, detector temperature: at a temperature of 280 c,

sample bottle: 80 ℃, valve box: 90 ℃, pipeline: 100 deg.C

The experimental steps are as follows:

(1) starting up a high performance gas chromatograph according to the chromatographic conditions;

(2) preparing a 50% triethylamine solution balance system: adding 1ml triethylamine sample and 1ml 1mol/L sodium hydroxide solution into a headspace bottle containing 0.6 gAR-grade sodium chloride, and pressing a cover to perform ultrasonic dissolution; balancing an instrument system and a chromatographic column by using 10 needles of triethylamine sample solution with the concentration of 50% in headspace sample injection;

(3) preparing a linear standard solution: analytically pure triethylamine 0.1230g is weighed precisely into a 50ml measuring flask and diluted to the mark with 1mol/L sodium hydroxide solution. Diluting according to the concentration shown in Table 1, precisely measuring 2ml, adding into a headspace bottle containing 0.6g of sodium chloride (AR grade), capping, and ultrasonically dissolving; performing high performance gas chromatography analysis on the linear standard solution to obtain a standard curve chart and a linear equation;

the results of the linear test (see table 1) show that the linear equation y of triethylamine is 1,030,137.3920x-83,039.3472, R²When the triethylamine content is 0.9993, the method proves that the triethylamine content is in a good linear relation;

(4) preparing a test solution: precisely measuring 1ml of a sample to be measured, adding 1ml of 1mol/L sodium hydroxide solution, placing into a headspace bottle containing 0.6g of sodium chloride (AR grade), capping, and ultrasonically dissolving;

(5) and (4) carrying out high-efficiency gas chromatography analysis on the test solution, recording a chromatogram and a peak area, and calculating by adopting an external standard method.

The chromatogram of the test sample is shown in FIG. 2: 11.917min is triethylamine peak, the rest is impurity peak. The peak-out time is proper, the theoretical plate number is 12789.157, the tailing factor is 1.031, and the separation degree from other impurity peaks is good.

Table 1: concentration and peak area of linear standard solution of triethylamine

Table 2: the concentration and peak area of the sample in this example

Test sample batch number	Dilution step	Peak area	Calculation results
				F-FG190613001 condensation concentration for 8h	1ml-2ml	859597.438	1.8g/L

Claims

1. A high performance gas chromatography detection method for triethylamine content in feed liquid is characterized in that:

the chromatographic conditions were as follows:

a chromatographic column: amine gas chromatographic column

sample bottle: 80 ℃; a valve box: 90 ℃; pipeline: 100 ℃;

the method comprises the following steps:

2. The detection method according to claim 1, characterized in that: in step (1), the sample injection is required to be carried out within 3 hours.

3. The detection method according to claim 1, characterized in that: the chromatographic column is Agilent CP-Volamine.

4. The detection method according to claim 1, characterized in that: and (3) balancing the triethylamine sample solution, the reference substance solution and the test sample solution in a valve box for 30min, and then injecting samples.