Nedaplatin impurity detection method

A detection method and technology of nedaplatin, applied in the field of HPLC analysis of nedaplatin, can solve the problems of affecting the separation of impurities, interference, affecting the accuracy of analysis, etc., to avoid potential safety hazards, improve durability and shorten the equilibration time. Effect

Active Publication Date: 2017-03-22
JIANGSU SIMCERE PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the above prior art, the HPLC analysis techniques of nedaplatin all adopt the method of isocratic elution. The disadvantage of these methods is that if multiple samples are analyzed at one time, the weak polar substance of the previous sample will not be washed out. Interference with the latter sample may affect the separation of impurities at the same time, and ultimately affect the accuracy of the entire analysis

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Experimental program
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Effect test

Embodiment 1

[0035] 1) Chromatographic conditions:

[0036] Instrument: Agilent1200HPLC

[0037] Chromatographic column: octadecylsilane bonded silica gel column (AQ-C18, 4.6×250mm, 5μm)

[0038] Mobile phase A: 0.5% potassium dihydrogen phosphate (pH 6.5 adjusted by ammonia)

[0039] Mobile Phase B: Acetonitrile

[0040] Time (min) Mobile phase A Mobile phase B 0973 5973 157030 15.1973 25973

[0041] Column temperature: 30℃

[0042] Flow rate: 0.8ml / min

[0043] Detection wavelength: 220nm

[0044] Injection volume: 10ul

[0045] Analysis time: record the chromatogram to 3 times the retention time of the principal component peak

[0046] Solvent: mobile phase A-mobile phase B (97:3)

[0047] 2) Sample preparation:

[0048] Take an appropriate amount of raw materials and add a solvent to make a solution containing 1.0 mg of nedaplatin per ml.

[0049] Take an appropriate amount of nedaplatin for injection and add a solvent to make a solution containing 1.0mg of nedaplatin per ml.

[0050] 3) Measurement...

Embodiment 2

[0052] 1) Chromatographic conditions:

[0053] Instrument: Agilent1200HPLC

[0054] Chromatographic column: octadecylsilane bonded silica gel column (4.6×250mm, 5μm)

[0055] Mobile phase A: 1% ammonium dihydrogen phosphate (triethylamine adjusted to pH 7.5)

[0056] Mobile phase B: methanol-acetonitrile (3:2)

[0057] Time (min) Mobile phase A Mobile phase B 0982 256040 25.1982 35982

[0058] Column temperature: 25℃

[0059] Flow rate: 0.6ml / min

[0060] Detection wavelength: 220nm

[0061] Injection volume: 10ul

[0062] Analysis time: record the chromatogram to 3 times the retention time of the principal component peak

[0063] Solvent: mobile phase A-mobile phase B (98: 2)

[0064] 2) Sample preparation:

[0065] Take an appropriate amount of raw materials and add a solvent to make a solution containing 1.0 mg of nedaplatin per ml.

[0066] Take an appropriate amount of nedaplatin for injection and add a solution containing 1.0 mg of nedaplatin per ml of solvent.

[0067] 3) Measurement...

Embodiment 3

[0069] 1) Chromatographic conditions:

[0070] Instrument: Agilent1200HPLC

[0071] Chromatographic column: octadecylsilane bonded silica gel column (4.6×250mm, 5μm)

[0072] Mobile phase A: 1% ammonium dihydrogen phosphate (triethylamine adjusted to pH 7.0)

[0073] Mobile phase B: methanol

[0074] Time (min) Mobile phase A Mobile phase B 0955 5955 256040 25.1982 30955

[0075] Column temperature: 40℃

[0076] Flow rate: 1.0ml / min

[0077] Detection wavelength: 220nm

[0078] Injection volume: 20ul

[0079] Analysis time: record the chromatogram to 3 times the retention time of the principal component peak

[0080] Solvent: mobile phase A-mobile phase B (95:5)

[0081] 2) Sample preparation:

[0082] Take an appropriate amount of raw materials and add a solvent to make a solution containing 1.5 mg of nedaplatin per ml.

[0083] Take an appropriate amount of nedaplatin for injection and add a solvent to make a solution containing 1.5 mg of nedaplatin per ml.

[0084] 3) Test results: The t...

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Abstract

The invention discloses a nedaplatin impurity HPLC (high-performance liquid chromatography) analysis method. According to the method, octadecylsilane chemically-bonded silica serves as a filling agent (AQ-C18 recommended), detection wavelength ranges from 205 nm to 222 nm, column temperature is 20-45 DEG C, and a mixed liquid of a buffer solution with a pH value of 6.0-8.5 and a polar organic solvent serves as a mobile phase. The method is characterized in that the mobile phase is used for eluting impurities in a nedaplatin sample by means of gradient elution, an initial ratio and a final ratio of the buffer solution with the pH value of 6.0-8.5 to the polar organic solvent is 100:0-90:10 and 90:10-60:40 respectively, and flow rate of the mobile phase is 0.5-1.0 ml / min; the mobile phase is prepared into a 0.5-2 mg / ml nedaplatin-containing solution; 5-20 microliters of sample solution is injected into a high-performance liquid chromatograph so as to record a chromatogram and conduct sample analysis. After the nedaplatin impurity HPLC analysis method is used, the main-peak theoretical plate number is increased remarkably, more impurities can be separated, and nedaplatin sample analysis accuracy is enhanced.

Description

Technical field [0001] The present invention relates to an HPLC analysis method of nedaplatin. Background technique [0002] Nedaplatin is an anti-tumor drug and was first approved for marketing in June 1995. It is used to treat head and neck tumors, small cell and non-small cell lung cancer, esophageal cancer, bladder cancer, testicular cancer, ovarian cancer, and cervical cancer. In clinical trials, it has been found that nedaplatin is effective against a wide range of solid tumors, better than cisplatin. It has an effective rate of more than 50% for esophageal cancer, about 20% higher than cisplatin, and an effective rate of more than 40% for cervical cancer. For these patients Provides new and effective clinical options. [0003] The retention time of the active component peak in nedaplatin is very short in the general chromatographic inspection system, and the impurities are difficult to separate. Not only the chromatographic inspection system has poor stability, reproducibil...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 王霞李薇
Owner JIANGSU SIMCERE PHARMA
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