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Method for measuring purity of trinexapac-ethyl standard substance

A standard substance and determination method technology, which is applied in the field of purity determination of trinexapac-ethyl agrotoxic chemical standard substances, can solve the problems of increasing the viscosity of the mobile phase, affecting the purity analysis results, increasing the system analysis pressure, etc., and achieving peak presentation properties. Good, repeatable and easy-to-operate effects

Inactive Publication Date: 2008-11-12
SHANGHAI INST OF MEASUREMENT & TESTING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following deficiencies in this method: (1) the preparation requirement of phosphoric acid aqueous solution is harsh, and only the aqueous solution of phosphoric acid can run normally when 0.1%, when the percentage content of phosphoric acid changes slightly, peak shape and peak-out time will occur (2) The ratio of the aqueous phase to the organic phase is 50:50, and the viscosity of the mobile phase increases, which increases the analysis pressure of the system; (3) Mass spectrometry is becoming the current food safety analysis method. The mainstream, such as phosphoric acid and other hard-to-volatilize mobile phases are not allowed to be used as eluting solutions for mass spectrometer detectors

Method used

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  • Method for measuring purity of trinexapac-ethyl standard substance
  • Method for measuring purity of trinexapac-ethyl standard substance
  • Method for measuring purity of trinexapac-ethyl standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Experimental equipment

[0038] Agilent1100 high performance liquid chromatography was selected, equipped with vacuum online degasser, quaternary gradient pump, 100 μL autosampler, multi-wavelength ultraviolet detector, column oven, and Agilent1100 chromatographic workstation.

[0039] 2. Test conditions

[0040] Chromatographic column: zorbax SB C18; column temperature 30°C; flow rate of mobile phase: 0.5mL / min; detection wavelength: 275nm; phase A of the mobile phase is formic acid: water = 0.2:100 (V / V), phase B is chromatography Pure grade acetonitrile, A phase: B phase=60:40 (V / V); Utilize mobile phase to prepare the solution of trinexapac-ethyl standard substance, make its absorption value on the ultraviolet detector 1200mAU; Injection volume: 10 μ L; After the instrument was stabilized, inject the sample, record the peak area, and calculate the purity of the trinexapac-ethyl standard substance by the area normalization method.

[0041] The peak area data of ...

Embodiment 2

[0045] 1. Experimental equipment

[0046] Described with embodiment 1.

[0047] 2. Test conditions

[0048] The flow rate of the mobile phase: 0.2mL / min; the A phase of the mobile phase is formic acid: water=0.05:100 (V / V), and the B phase is chromatographically pure grade methanol, A phase: B phase=80:20 (V / V ); Utilize mobile phase to prepare the solution of trinexapac-ethyl standard substance, make its absorption value on the ultraviolet detector be 2500mAU; Injection volume: 5 μ L; All the other conditions are as described in embodiment 1.

[0049] The peak area data of this embodiment are shown in Table 2, and the purity result calculated by the area normalization method is 98.7%, and its typical chromatogram is shown in figure 2 shown.

[0050] The peak area data of table 2 embodiment 2

[0051]

Embodiment 3

[0053] 1. Experimental equipment

[0054] Described with embodiment 1.

[0055] 2. Test conditions

[0056] The flow rate of the mobile phase: 0.8mL / min; the A phase of the mobile phase is formic acid: water=0.1:100 (V / V), and the B phase is chromatographically pure grade acetonitrile, A phase: B phase=20:80 (V / V ); Utilize mobile phase to prepare the solution of trinexapac-ethyl standard substance, make its absorption value on the ultraviolet detector 1600mAU; Injection volume: 50 μ L; All the other conditions are as described in embodiment 1.

[0057] The peak area data of this embodiment are shown in Table 3, and the purity result calculated by the area normalization method is 98.8%, and its typical chromatogram is shown in image 3 shown.

[0058] The peak area data of table 3 embodiment 3

[0059]

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Abstract

The invention discloses a purity determination method of a trinexapac ethyl standard substance; the method adopts octadecyl silane to bond silica gel chromatographic column, and uses high performance liquid chromatograph with an ultraviolet detector to measure the peak areas, and finally the purity is calculated according to normalization; wherein, the mobile phase, phase A, is formic acid: water =0.05: 100-0.2: 100, phase B is acetonitrile or methanol, and the proportion between phase A and phase B is 80: 20-20: 80. The absorption value of the solution of trinexapac ethyl standard substance at the ultraviolet detector is 1000-3000mAU, while the wavelength of the ultraviolet detector is 275nm. The purity determination method of trinexapac ethyl standard substance provided by the invention is characterized by good peak presentation, high resolution, good repeatability and convenient operation, and can accurately, stably and rapidly determine the purity of trinexapac ethyl standard substance, which supplies effective guarantee for the control of residual of trinexapac ethyl in farm products.

Description

technical field [0001] The invention relates to a method for measuring the purity of a standard substance of an agricultural toxic chemical, in particular to a method for measuring the purity of a standard substance of a trinexapac-ethyl agricultural toxic chemical. Background technique [0002] As the world pays more attention to food safety issues, the detection of toxic and harmful chemicals in agricultural products has also been put on the agenda. However, the isomers of such substances are complex, and the degradation and decomposition speed are fast, which brings difficulties to the detection work. . How to realize the mutual recognition of the test results of toxic and harmful chemicals in agricultural products in various laboratories, the key issue is to develop high-quality reference materials, and the determination of the purity of such reference materials has become a key technology. In 2006, Japan's "positive list system" involved the management of all toxic and...

Claims

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Application Information

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IPC IPC(8): G01N30/86G01N30/02
Inventor 田玉平郝玉红王东辉
Owner SHANGHAI INST OF MEASUREMENT & TESTING TECH
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