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Automatic headspace sampling gas chromatography method for determining chloroethane and chloroform residual in chlortetracycline hydrochloride

A technology of gas chromatography and aureomycin hydrochloride, which is applied in the field of automatic headspace sampling gas chromatography, can solve the problems of manpower consumption, material resources, long detection time, low sensitivity, etc., to save carrier gas, reduce detection cost, The effect of improving test efficiency

Inactive Publication Date: 2018-02-23
金河生物科技股份有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] At present, the commonly used detection method of ethyl chloride is detected by gas chromatography, and the method of detecting ethyl chloride and chloroform in the HG / T2662-95 standard and GBZ / T160.45-2007 "Determination of Haloalkane Compounds of Air Toxic Substances in the Workplace" They are all detected with stainless steel packed columns, the operation is cumbersome, and the detection time is long, the sensitivity is low, and it consumes manpower and material resources. Therefore, it is necessary to improve and perfect the detection methods of ethyl chloride and chloroform

Method used

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  • Automatic headspace sampling gas chromatography method for determining chloroethane and chloroform residual in chlortetracycline hydrochloride
  • Automatic headspace sampling gas chromatography method for determining chloroethane and chloroform residual in chlortetracycline hydrochloride
  • Automatic headspace sampling gas chromatography method for determining chloroethane and chloroform residual in chlortetracycline hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Precision Test

[0064] 1. Instrument precision test

[0065] The precision of the instrument is the embodiment of the repeatability of the instrument. Accurately measure 10mL of the above-mentioned mixed control solution, place it in a 20mL headspace bottle, seal the bottle, and prepare 6 copies in this way, and set them under the above-mentioned gas chromatography conditions and headspace sampling parameters respectively. Under measure, calculate the average value and relative standard deviation (RSD) of ethyl chloride and chloroform peak area, the results are shown in Table 1, wherein the gas chromatogram of parallel experiment group 1 is as follows figure 1 shown.

[0066] Table 1 Instrument precision test data statistics

[0067] serial number

Area of ​​ethyl chloride

Chloroform peak area

1

8108

29644

2

7832

30715

3

8301

29736

4

7794

30402

5

8284

29543

6

7956

29956

ave...

Embodiment 2

[0078] accuracy test

[0079] Accuracy is the closeness between the measured value and the true value, and the accuracy of the method is usually expressed by the recovery rate. Add ethyl chloride and chloroform to aureomycin hydrochloride samples by standard addition method to prepare solutions of three concentration levels, detect the concentration of the standard addition solution, and calculate the recovery rate of each concentration.

[0080] 1. Preparation of recovery standard solution

[0081] Accurately measure 5mL, 10mL and 15mL of the above-mentioned mixed control solutions respectively, place them in a 100mL volumetric flask, add water to dilute to the mark, and obtain 50% recovery solution, 100% recovery solution and 150% recovery solution respectively, and then take 10mL50 %, 100% and 150% of the recovery solution, each 3 parts, were added to 20ml headspace vials, and then 0.05g chlortetracycline hydrochloride sample was added to 9 headspace vials, after the chlor...

Embodiment 3

[0086] Linearity and range determination

[0087] Precisely measure 1mL, 2mL, 5mL, 10mL, 15mL, 20mL, 40mL, 50mL of the mixed standard stock solution respectively and place them in a 100mL volumetric flask, dilute to the mark with water to obtain a series of mixed standard solutions of 8 concentration levels, ethyl chloride and Chloroform concentrations were approximately 0.01 μg / mL, 0.02 μg / mL, 0.05 μg / mL, 0.10 μg / mL, 0.15 μg / mL, 0.20 μg / mL, 0.40 μg / mL, 0.50 μg / mL.

[0088] Get each 10mL of above-mentioned series mixed contrast solution, place respectively in the headspace bottle of 20mL, seal the bottle, measure respectively according to above-mentioned this gas chromatographic condition and headspace sampling parameter setting, record the peak area of ​​ethyl chloride and chloroform, The results are shown in Table 4, carry out linear regression analysis with the amount of ethyl chloride and chloroform detected in this series of mixed contrast solutions and the corresponding ...

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Abstract

The invention relates to an automatic headspace sampling gas chromatography method for determining chloroethane and chloroform residual in chlortetracycline hydrochloride and belongs to the technicalfield of analysis detection. The method has gas chromatography conditions of a sampling temperature of 25 DEG C, a column temperature of 40 DEG C, nitrogen gas as carrier gas, a carrier gas flow of 60mL / min, a detector temperature of 250 DEG C, a split ratio of 5: 1, a sampling volume of 1.0mL, air velocity of 250mL / min and operation time of 12min, and headspace sampling parameters of a constant temperature oven temperature of 60 DEG C, sample constant temperature time of 30min, sample pressing time of 2.0min, pressing balance time of 0.1min, leading time of 0.1min, sampling time of 1.0min anda sampling amount of 1mL. The method utilizes automatic headspace sampling, optimizes a sampling temperature and carrier gas flow, provides a test precision and sensitivity, shortens the existing detection time 26min to 12min, improves test efficiency, saves carrier gas, realizes simultaneous detection of chloroform and chloroethane, further improves test efficiency and reduces a detection cost.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to an automatic headspace sampling gas chromatography method for determining residual ethyl chloride and chloroform in aureomycin hydrochloride. Background technique [0002] Ethyl chloride is listed as a first-class solvent in ICH Q3C, which can cause cancer and is harmful to humans and the environment. In raw materials, the residue must be limited within 5ppm. Chloroform, listed as a second-class solvent, is an animal carcinogenic solvent, and the residue must be controlled within 60ppm. With the gradual improvement of people's awareness of residues in food, medicine and air, more stringent requirements are put forward for the residue detection method. Since the residues of ethyl chloride and chloroform are detected in trace amounts, the sensitivity and detection limit of the method are required. very high. [0003] At present, the commonly used detect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/68G01N30/24
CPCG01N30/02G01N30/24G01N30/68
Inventor 谢昌贤秦定宇胡子夜金玲玲刘运添云喜报王鹏飞
Owner 金河生物科技股份有限公司
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