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Method for detecting kasugamycin by high performance liquid chromatography

A high-performance liquid chromatography and kasugamycin technology, which is applied in the field of high-performance liquid chromatography for detecting kasugamycin, can solve the problems of inconvenient analysis work, damaged chromatographic column, complicated operation and the like, and achieves simple preparation, rapid and accurate detection and detection. low cost effect

Pending Publication Date: 2020-07-28
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method produces HF gas in the derivatization reaction, which is highly toxic. In order to prevent the derivatives from being decomposed, special refrigeration equipment is required. The method is complicated to operate and requires many steps, time-consuming and laborious; The element is not retained on the chromatographic column, and ion pairing is required as the mobile phase. In addition to causing damage to the chromatographic column, the operation is also complicated, which brings inconvenience to the analysis work

Method used

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  • Method for detecting kasugamycin by high performance liquid chromatography
  • Method for detecting kasugamycin by high performance liquid chromatography
  • Method for detecting kasugamycin by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Chromatographic conditions:

[0034] Chromatographic column: Agela Venusil HILIC (Agela, 4.6mm×150mm, 5μm); mobile phase: acetonitrile: ammonium formate-formic acid buffer solution = 70:30 (volume ratio); elution method: isocratic elution; flow rate: 1.0mL / min; detection wavelength: 220-245nm; column temperature: 40°C; injection volume: 10μL; detector adopts diode array detector, elution time: 8min.

[0035] The specific operation steps are:

[0036] (1) Weigh 0.0629g of kasugamycin standard substance, place it in a 100ml volumetric flask, add 90ml of water phase, dissolve the standard substance by ultrasonic vibration, cool to water temperature, dilute with water phase to the mark, shake well, and obtain kasugamycin standard The product solution is ready for use;

[0037] (2) Weigh 0.0649g of the kasugamycin sample to be tested, place it in a 100ml volumetric flask, add 90ml of the water phase, dissolve the sample to be tested by ultrasonic vibration, cool to water t...

Embodiment 2

[0052] According to the detection method of embodiment 1, the composition of mobile phase has been studied, and the relation of concrete mobile phase composition and peak time is as follows table 2:

[0053] Table 2-Relationship between mobile phase composition and peak elution time

[0054]

[0055]

[0056] According to the detection spectrum, it is found that the detection wavelength range of the present invention is 220-245nm, and has the following characteristics. With the red shift of the wavelength, the peak area of ​​kasugamycin has a downward trend, and with the blue shift of the wavelength, the baseline will become worse.

Embodiment 3

[0058] In order to verify the feasibility and accuracy of the detection method of the present invention, now take Example 1 as an example to carry out the following verification test:

[0059] (1) The precision and accuracy of the sample

[0060] Chromatographic conditions:

[0061] Chromatographic column: Agela Venusil HILIC (Agela, 4.6mm×150mm, 5μm); mobile phase: acetonitrile: ammonium formate-formic acid buffer solution = 70:30 (volume ratio); flow rate: 1.0mL / min; detection wavelength: 220 -245nm; Column temperature: 40°C; Injection volume: 10μL; The detector uses a diode array detector;

[0062] Under the above-mentioned stable chromatographic conditions, the kasugamycin sample to be tested in Example 1 with the same content was tested repeatedly for 6 times to test the precision of the method. The precision experiment result of the present invention is as follows table 3:

[0063] Table 3 - Results of precision experiments

[0064]

[0065] From the experimental ...

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Abstract

The invention relates to a method for detecting kasugamycin by high performance liquid chromatography, and belongs to the technical field of pharmaceutical analysis. Chromatographic conditions of themethod are as follows: a chromatographic column is Igeerre Virusil HILIC (Agela, 4.6mm*150mm, 5[mu]m), a mobile phase is an organic phase-water phase, an elution mode is isocratic elution, the flow rate is 1.0mL / min;, the detection wavelength is 220-245 nm, the column temperature is 40 DEG C, the sample size is 10[mu]L, a diode array detector is adopted as the detector, and isocratic elution is carried out. According to the method, an ion pair is prevented from being used as a mobile phase, so that the chromatographic column is prevented from being damaged; and kasugamycin can be effectively retained, so that interference of solvent peaks, inverted peaks and impurity peaks is avoided, and rapid and accurate detection can be realized.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting kasugamycin by high performance liquid chromatography. Background technique [0002] Kasugamycin is a kind of low toxicity, systemic fungicide. It has excellent control and treatment effects on rice blast. It is effective in preventing watermelon bacterial angular spot, peach tree gummosis, scab, perforation and other diseases. [0003] Because of its high polarity and non-characteristic ultraviolet absorption, kasugamycin hydrochloride is not retained in the liquid chromatography column, and often emerges simultaneously with inverted peaks, solvent peaks, and impurity peaks, which brings difficulties to analysis and detection. [0004] The structural formula of kasugamycin hydrochloride is as follows: [0005] [0006] Most of the existing detection methods require a large amount of pretreatment to modify a hydrophobic chromophore on the molecu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74G01N2030/324
Inventor 董艳艳于连友张道磊张元珍
Owner JINGBO AGROCHEM TECH CO LTD
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