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Method for detecting isatin anhydride

A technology of isatoic anhydride and a detection method, applied in the detection field of bentazone intermediates, can solve the problems of difficulty in controlling the completeness of esterification, difficulty in guaranteeing accuracy, long required time, etc., and achieves reduction of detection cost and improvement of accuracy , the separation effect satisfies the effect

Inactive Publication Date: 2008-06-25
ANHUI FENGLE AGROCHEM
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Problems solved by technology

Because isatoic anhydride is easy to decompose when heated, it cannot be directly analyzed by gas chromatography. It needs to be esterified first. The esterification reaction requires a long time and a certain temperature requirement, and it is difficult to control the complete degree of esterification.
Therefore, this method is not only complicated and time-consuming, but also difficult to guarantee accuracy.

Method used

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  • Method for detecting isatin anhydride
  • Method for detecting isatin anhydride
  • Method for detecting isatin anhydride

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Experimental program
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Embodiment Construction

[0027] 1. Reagents and solutions

[0028] Methanol: chromatographically pure;

[0029] Glacial acetic acid: AR;

[0030] Water: newly steamed twice distilled water;

[0031] Isatoic anhydride standard sample: known content ≥ 99.0%;

[0032] 2. Instrument

[0033] High performance liquid chromatography: with adjustable wavelength ultraviolet detector;

[0034] Zhejiang University N2000 chromatography workstation;

[0035] Chromatographic column: 250mm×4.6mm stainless steel column, filled with ODS filler, particle size 5μm;

[0036] Ultrasonic cleaner;

[0037] Filter: The pore size of the filter membrane is about 0.45 μm;

[0038] Injector: 10 μl.

[0039] 3. Operating conditions of high performance liquid chromatography

[0040] Mobile phase: Methanol + water (adjusted to pH = 4 with glacial acetic acid first) = 65 + 35 (v / v), the mobile phase is filtered through a microporous membrane, and used after ultrasonic degassing.

[0041] Flow rate: 0.6ml / min;

[0042] Col...

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Abstract

A detection method for isatoic anhydride belongs to the pesticide technical field, and aims to provide a detection method for isatoic anhydride with simple operation and capable of increasing detection speed and detection accuracy. The method includes the following technical points that: isatoic anhydride sample and standard substance are respectively dissolved by methanol at room temperature condition and then constant volume process is completed; an ODS stainless steel column and an ultraviolet detector are adopted, and the solution of methanol and water is taken as mobile phase with the flow rate controlled at about 0.6ml / min; detection wavelength is adjusted to 254nm, and high efficient liquid phase chromatogram separation and quantification of the isatoic anhydride in the sample is completed. Due to changing the prior indirect gas chromatography to direct liquid chromatography and replacing the gas phase chromatogram detection method adopted after derivation reaction by direct liquid phase detection, the method greatly simplifies the detection method for isatoic anhydride and substantially increases detection speed; meanwhile, because derivation reaction is reduced, the invention reduces detection cost and increases detection accuracy at the same time.

Description

Technical field: [0001] The invention relates to a detection method of a bentazone intermediate, in particular to a detection method of isatoic anhydride. Background technique: [0002] Benedazone is a contact-type selective post-emergence herbicide, used for stem and leaf treatment at the seedling stage, and works through leaf contact. The active ingredients are metabolized to the weakly active sugar conjugates in the tolerant crops for detoxification, which is safe for crops. It is an ultra-efficient dryland herbicide suitable for annual and perennial grass weeds such as sugar beet, cotton, peanut, soybean, etc., and has a broad market prospect. And isatoic anhydride is a key intermediate for the synthesis of bentazone, whether its reaction is complete and its quality is reliable directly determines the quality and cost of bentazone. [0003] The molecular formula of the compound: C 8 h 5 NO 3 [0004] CAS registration number: 118-48-9 [0005] Chemical name: 2-(4'-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 赵邦斌金劲松赵国平缪莉吴燕王飞
Owner ANHUI FENGLE AGROCHEM
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