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Method for detecting dimethyl sulfate contained in ciprofloxacin hydrochloride

A technology of ciprofloxacin hydrochloride and dimethyl sulfate, which is applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of poor specificity and precision, high polarity of dimethyl sulfate, insufficient sensitivity, etc. and good precision, good precision, good specificity

Active Publication Date: 2020-10-30
武汉九州钰民医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Spectrophotometry is quantified by colorimetry, which has poor specificity and precision; dimethyl sulfate is very polar and does not have sensitive UV-absorbing groups, and liquid chromatography detection needs to be detected after derivatization, which is cumbersome to operate. Poor specificity and precision; using gas chromatography hydrogen flame ionization detector, the sensitivity is not enough

Method used

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  • Method for detecting dimethyl sulfate contained in ciprofloxacin hydrochloride
  • Method for detecting dimethyl sulfate contained in ciprofloxacin hydrochloride
  • Method for detecting dimethyl sulfate contained in ciprofloxacin hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] A detection method for dimethyl sulfate contained in ciprofloxacin hydrochloride, comprising:

[0048] 1) adopt the gas chromatograph that is equipped with FPD detector to detect blank solution, multiple reference substance solutions with different concentrations and test solution respectively; Wherein, blank solution, multiple reference substance solutions with different concentrations and supply The test solutions are as follows:

[0049] Blank solution: ethyl acetate

[0050] Reference substance stock solution: Take an appropriate amount of dimethyl sulfate, weigh it accurately, add ethyl acetate to quantitatively dilute it to make about 0.1 mg of dimethyl sulfate per 1 mL, and shake well. (0.1mg / mL)

[0051] Reference substance solution:

[0052] 600% reference substance solution: Accurately measure 60 μL of the reference substance stock solution, put it in a 10mL measuring bottle, dilute to the mark with ethyl acetate, and shake well. (0.60μg / mL)

[0053] 400%...

Embodiment 2

[0072] Example 2: Sensitivity

[0073] Limit of quantitation solution 1-6: Take an appropriate amount of dimethyl sulfate, weigh it accurately, add ethyl acetate to quantitatively dilute to make about 0.06 μg of dimethyl sulfate per 1 mL, and shake well. (0.06μg / mL)

[0074] Detection limit solution 1-2: Take an appropriate amount of dimethyl sulfate, weigh it accurately, add ethyl acetate to quantitatively dilute to make about 0.03 μg of dimethyl sulfate per 1 mL, and shake well. (0.03μg / mL)

[0075] A gas chromatograph equipped with an FPD detector was used to detect the quantitative limit solution 1-6 and the detection limit solution 1-2, and the detection method and conditions were the same as in Example 1.

[0076] The signal-to-noise ratio of the limit of quantitation solution is shown in the table below:

[0077] Table 1:

[0078]

[0079]

[0080] The signal-to-noise ratio of the detection solution is shown in the table below:

[0081] Table 2:

[0082] ...

Embodiment 3

[0083] Example 3: Precision

[0084] Control solution 1-6: Take an appropriate amount of dimethyl sulfate, weigh it accurately, add ethyl acetate to quantitatively dilute to make about 0.1 μg of dimethyl sulfate per 1 mL, and shake well. (0.1μg / mL)

[0085] Test product 1-6: Accurately weigh 0.5g of ciprofloxacin hydrochloride, put it into a 10mL stoppered glass centrifuge tube, accurately add 5mL of ethyl acetate, ultrasonicate for 15 minutes, centrifuge at 4000 rpm, take the supernatant and filter , continued filtrate as the test solution.

[0086] Adopt the gas chromatograph that is configured with FPD detector to contrast solution 1-6, need testing sample 1-6 detect, detection method and condition are with embodiment 1, and detection result is as shown in the table below:

[0087] table 3:

[0088]

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Abstract

The invention provides a method for detecting dimethyl sulfate contained in ciprofloxacin hydrochloride. The method comprises the following step: detecting a ciprofloxacin hydrochloride test solutionby adopting a gas chromatograph provided with an FPD detector, a chromatographic column of the gas chromatograph being a chromatographic column filled with polyethylene glycol, the initial column temperature being 70 + / -1 DEG C, and the flow rate of the ciprofloxacin hydrochloride test solution being 2.0 + / -0.05 mL / min. The detection method provided by the invention does not need derivatization, and has the advantages of no interference, high signal-to-noise ratio, good precision and simple detection operation.

Description

technical field [0001] The invention relates to a detection method for dimethyl sulfate contained in ciprofloxacin hydrochloride. Background technique [0002] Ciprofloxacin is a synthetic third-generation quinolone antibacterial drug with broad-spectrum antibacterial activity and good bactericidal effect. The antibacterial activity against almost all bacteria is 2 to 4 times stronger than that of norfloxacin and enoxacin. Enterobacter, Pseudomonas aeruginosa, Haemophilus influenzae, Neisseria gonorrhoeae, Streptococcus, Legionella, Staphylococcus aureus have antibacterial effect. [0003] Ciprofloxacin hydrochloride tablets are clinically used for sensitive bacteria: 1. Genitourinary system infection, including simple and complicated urinary tract infection, bacterial prostatitis, Neisseria gonorrhoeae urethritis or cervicitis (including caused by enzyme strains). 2. Respiratory tract infection, including acute attack of bronchial infection and lung infection caused by se...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/60G01N30/64G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/6078G01N30/64G01N30/8675G01N2030/324G01N2030/685Y02A50/30
Inventor 刘均均范昭泽余艳平顿伟张璐罗亚琼柳少群许勇
Owner 武汉九州钰民医药科技有限公司
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