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Gas Chromatographic Detection Method of 1-Bromo-2-Propanol in Urine

A gas chromatography and gas chromatography technology, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of complex metabolism of 1-BP, and achieve the effects of high repeatability, simple operation and stable peak output.

Inactive Publication Date: 2016-06-01
缪荣明
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The metabolic process of 1-BP is more complex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] TraceGCUltra gas chromatograph, equipped with AutoinjectorAI3000 autosampler (Finnigan, USA); hydrogen generator (QL type, Jinan Applied Chemical Technology Development Co., Ltd.); low-noise air pump (GA3000, Beijing Zhongxing Huili Technology Development Co., Ltd.) ; Auto-sampling vials (Agilent, USA), solvent desorption activated carbon tubes (100 / 50 mg, Nantong Jinnanbo Instrument Hardware Factory, Jiangsu Province).

[0021] Accurately weigh 50.00 mg of 1-bromo-2 propanol, CS 2 After dissolving, dilute to 50mL volumetric flask, this solution is 1.0mg / mL 1-BP stock solution. Store in 4°C refrigerator for later use. Pipette an appropriate amount of stock solution of 1-bromo-2-propanol with CS 2 Dilute the standard series to 2.50, 10.00, 50.00, 100.00, 500.00 μg / mL, use gas chromatography to detect the peak values ​​of different concentrations of 1-bromo-2 propanol solution, take 1-bromo-2 propanol solution as the abscissa, peak The standard curve obtained by fittin...

Embodiment 2

[0031] Embodiment 2 accuracy checking

[0032]Using the method in Example 1, collect the urine of ordinary adults (those who have not been exposed to 1-BP), and test to confirm that there is no 1-bromo-2-propanol in the urine components. Divide the urine into 01~09 groups, add 1-bromo-2 propanol of different quality in each group of urine, make 1-bromo-2 propanol urine of different concentrations, with the method in embodiment 1, to 1-bromo-2 propanol was detected in each group of urine, and the experimental results are shown in Table 1.

[0033] Table 1:

[0034] Numbering

[0035] It can be seen from the results in the table that the detection accuracy of this method is high, and the error is less than 5 per thousand, which can be used for the precise measurement of 1-bromo-2-propanol in urine.

[0036] 03 groups of samples were used for 5 injection tests, and the recorded results are shown in Table 2.

[0037] Table 2

[0038] Number of injections

...

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Abstract

The invention discloses a gas chromatography detection method for 1-bromine-2 propyl alcohol in urine. The method comprises the following steps: absorbing 2.0 mL of urine sample into a 10 mL centrifuge tube, adding 1.5 mL of a sulfuric acid solution, shaking uniformly, placing into boiling water bath, heating for 8 hours, taking out, cooling to the room temperature, adding 5 mL of a sodium hydroxide solution, mixing uniformly, adding 2 mL of methyl benzene, shaking for 2 min, centrifuging at 1500 r / min for 10 min, taking out 1.5 mL of methyl benzene layer, placing into another centrifuge tube, adding 20 mL of heptafluorobutyric anhydride, shaking for 2 min, settling for 5 min, adding 1 mL of a buffer solution, shaking for 2 min, removing redundant heptafluorobutyric anhydride, settling for 2 min, taking the methyl benzene layer to perform sample introduction detection, recording the peak value, and calculating so as to obtain the concentration of the 1-bromine-2 propyl alcohol in the urine. According to the invention, the accuracy is high, the error is less than 0.5%, the operation is simple, the sensitivity is high, the detection limit is 2.5 [mu]g / mL, the peak is stable, and the repeatability is high.

Description

technical field [0001] The invention relates to a gas chromatography detection method for 1-bromo-2 propanol in urine, belonging to the technical field of chemical analysis. Background technique [0002] Bromopropane (1-bromopropane, 1-BP), also known as bromide n-propane (n-propylbromide, nPB). It is a colorless and slightly sweet liquid with a relative molecular mass of 123.00, a density of 1.35g / m², a melting point of -110.0°C and a boiling point of 71.0°C. Slightly soluble in water, soluble in acetone, benzene, chloroform, miscible with ethanol and ether. Since 1-BP has the characteristics of low toxicity, high efficiency and no damage to the ozone layer, it has become an ideal substitute for ozone depleting substances (ODS) cleaning agents since the late 1990s. At present, I-BP, as an efficient and environmentally friendly cleaning agent, is widely used in the cleaning process of various greases, fluxes, hardware electronics, precision machinery, clothing dry cleaning...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 缪荣明
Owner 缪荣明
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