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Method for simultaneously detecting contents of praziquantel, clofenoxine and milbemycin oxime

A technology of milbexime and praziquantel, which is applied in the field of chemical analysis, can solve problems such as undisclosed detection methods of the content, and achieve the effects of simple detection methods, cost reduction, and time saving

Active Publication Date: 2022-04-05
上海汉维生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, oral pet deworming medicines with these three ingredients have appeared on the overseas market, but the detection method of its content has not been made public

Method used

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  • Method for simultaneously detecting contents of praziquantel, clofenoxine and milbemycin oxime
  • Method for simultaneously detecting contents of praziquantel, clofenoxine and milbemycin oxime
  • Method for simultaneously detecting contents of praziquantel, clofenoxine and milbemycin oxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Example 1: System Suitability

[0100] Chromatography program

[0101] Do system suitability test according to the requirements of the analysis method. After the system is balanced, take 20 μL of the reference substance solution, inject it into the liquid chromatograph, and record the chromatogram. Advanced 5 needles Std-1, calculate the relative standard deviation (RSD), then enter 2 needles Std-2, use Std-1 to calculate the accuracy of Std-2, as shown in Table 7.

[0102] Table 7

[0103]

[0104]

[0105] The formula for calculating the recovery rate of Std-2 with Std-1:

[0106]

[0107] A Std-1 =The average value of the peak area of ​​each component in the Std-1 chromatogram.

[0108] A Std-2 =The average value of the peak area of ​​each component in the Std-2 chromatogram.

[0109] C Std-1 =Concentration of each component in Std-1.

[0110] C Std-2 =Concentration of each component in Std-2.

[0111] The system suitability test results are shown...

Embodiment 2

[0122] Example 2: Specificity

[0123] Specificity will be confirmed by the interference of the blank and the interference of degraded impurities.

[0124] Blank solution (diluent): Inject acetonitrile directly.

[0125] Sample: Weigh the raw material of praziquantel (source: Hebei Jiayi Pharmaceutical Co., Ltd., batch number: JYC-200402), the new raw material of chlorophene (source: Zhejiang Haisheng, batch number: N181101), the raw material of milbexime (source: Zhejiang Hisun Pharmaceutical Co., Ltd., batch number: 4037-A180405U) constituted a mixture with a similar weight of 14.2 mg as a sample for the destruction test.

[0126] Acid degradation: Weigh the sample, put it in a 100mL measuring bottle, add 5.0mL, 1mol / L hydrochloric acid solution, leave it at room temperature for 5min, adjust the pH value to 7.0 with 1mol / L sodium hydroxide solution, cool to room temperature, Dilute to the mark with diluent, shake well, that is.

[0127] Alkali degradation: Weigh the sampl...

Embodiment 3

[0135] Example 3: Linear

[0136] The linearity studies of praziquantel, clofenacine and milbexime in the assay ranged from 60-140% concentration. Carry out the linearity study test as follows.

[0137] Test Procedures and Results Processing

[0138] With the concentration (μg / mL) as the abscissa and the peak area as the ordinate, draw the standard curve y=ax+b.

[0139] Calculate the correlation coefficient r of the standard curve.

[0140] Calculate the linear deviation Bias%: that is, the intercept b is relative to the peak area y at 100% concentration 100％ percentage.

[0141]

[0142] Calculate the mean response factor (MRF):

[0143]

[0144] The linearity test results are shown in Table 13 to Table 15, Figure 9 to Figure 11 shown.

[0145] Table 13

[0146]

[0147]

[0148] Table 14

[0149]

[0150]

[0151] Table 15

[0152]

[0153] In summary, it can be seen that the repeatability RSD of three injections at each concentration n＝3 Al...

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Abstract

The invention provides a method for simultaneously detecting contents of praziquantel, clofenoxine and milbemycin oxime, which comprises the following steps: firstly preparing a blank solution, then preparing a test solution containing praziquantel, clofenoxine and milbemycin oxime, finally preparing a system applicability test solution, respectively injecting into a liquid chromatograph, and recording chromatograms under ultraviolet wavelength; according to the method, acetonitrile is taken as a diluent, octadecylsilane chemically bonded silica is taken as a chromatographic column in a liquid chromatograph, gradient elution is carried out, the flow rate is 1.0 mL / min, the column temperature is 30 DEG C, the ultraviolet detection wavelength is 230 nm, and the sample size is 20 mu L; the mobile phase A is a phosphoric acid solution with the content of 10-30 wt%, and the mobile phase B is acetonitrile with the content of 70-90 wt%; the detection method provided by the invention is simple and convenient, saves time, reduces cost, has good specificity, accuracy, linearity, durability and precision, and is suitable and accurate for detecting the content of the three components, so that the detection method can be used for daily detection of the pet medicine.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and in particular relates to a method for simultaneously detecting the content of three components of praziquantel, clofenacine and milbexime. Background technique [0002] Praziquantel is a pyrazinoquinoline derivative with anthelmintic activity, which was developed by Bayer in the 1970s and is a broad-spectrum anti-fluke and tapeworm drug. [0003] [0004] The mechanism of action of praziquantel has not been fully elucidated, and the mainstream view is that praziquantel may change the parasite’s response to Ca 2+ The permeability of the worm body promotes its internal flow, which leads to the activity of the worm body and muscle contraction, so that it cannot be well adsorbed on the blood vessel wall; The immune system recognizes it, attracting immune cells to attack it. Therefore, the insecticidal mechanism of praziquantel can be summarized as two parts: the direct effect of th...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
CPCY02A50/30
Inventor 宋毓
Owner 上海汉维生物医药科技有限公司
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