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A high performance liquid chromatography detection method for zoledronic acid and impurities of the zoledronic acid

A high-performance liquid chromatography and zoledronic acid technology, which is applied in the field of high-performance liquid chromatography detection of zoledronic acid raw materials and impurities thereof, can solve the problems of limited number of separated impurities, tailing of chromatographic peaks, and inaccurate content detection. and other problems to achieve the effect of good separation and good reproducibility

Active Publication Date: 2019-08-23
SICHUAN KELUN PHARMA RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN201610794684.6 discloses a method for detecting related substances in zoledronic acid injection by high performance liquid chromatography, using octadecylsilane bonded silica gel as a filler, and the mobile phase includes disodium hydrogen phosphate, tetrahexylammonium hydrogen sulfate, methanol and acetonitrile, although the reversed-phase ion-pair reagent used in this method solves the problem of compound retention to a certain extent, the problem of chromatographic peak shape tailing cannot be effectively solved, resulting in poor separation of the main peak and impurity peaks, and the number of separated impurities is limited. Content detection is not accurate

Method used

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  • A high performance liquid chromatography detection method for zoledronic acid and impurities of the zoledronic acid
  • A high performance liquid chromatography detection method for zoledronic acid and impurities of the zoledronic acid
  • A high performance liquid chromatography detection method for zoledronic acid and impurities of the zoledronic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0045] A high-performance liquid chromatography detection method for zoledronic acid and impurities thereof, comprising the following chromatographic conditions:

[0046] Stationary phase: Shiseido Capcell Pak C8 DD (250*4.6mm, 5μm);

[0047] Mobile phase: [10mmol / L sodium pyrophosphate + 20mmol / L tetrabutylammonium bisulfate (pH8.0)], methanol, 3.6mg / mlEDTA solution, the volume ratio is 900:100:0.5;

[0048] Flow rate: 1.0ml / min, detection wavelength: 215nm, column temperature: 30°C, injection volume: 20μl.

[0049] Blank solvent: Take a blank solvent for sample analysis, and the blank solvent will not interfere with the detection of each impurity peak.

[0050] Reference substance solution: Accurately weigh the appropriate amount of impurity 1, impurity 2, impurity 3, impurity 4, impurity 5, and impurity 6 reference substances respectively, add diluent to dissolve and dilute to make a reference substance solution of appropriate concentration, inject samples for analysis, T...

Embodiment 2

[0058] A high-performance liquid chromatography detection method for zoledronic acid and impurities thereof, comprising the following chromatographic conditions:

[0059] Stationary phase: Shiseido Capcell Pak C8 DD (250*4.6mm, 5μm);

[0060] Mobile phase: [10mmol / L sodium pyrophosphate + 20mmol / L tetrabutylammonium bisulfate (pH8.0)], methanol, 3.6mg / mlEDTA solution, the volume ratio is 850:150:0.5;

[0061] Flow rate: 1.0ml / min, detection wavelength: 215nm, column temperature: 30°C, injection volume: 20μl.

[0062] System suitability solution 2: take appropriate amount of impurity 1, impurity 2, impurity 3, impurity 4 and zoledronic acid reference substance, add mobile phase to dissolve and dilute to make each 1ml contains about 1.2 μg of each impurity, zoledronic acid About 0.8mg of the mixed solution.

[0063] System suitability solution 2 was tested as above. HPLC spectrum see figure 2 , and the test results are shown in Table 4.

[0064] The detection result of tab...

Embodiment 3

[0068] A high-performance liquid chromatography detection method for zoledronic acid and impurities thereof, comprising the following chromatographic conditions:

[0069] Stationary phase: Shiseido Capcell Pak C8 DD (250*4.6mm, 5μm);

[0070] Mobile phase: Condition ①: The volume ratio of [10mmol / L sodium pyrophosphate + 20mmol / L tetrabutylammonium bisulfate (pH7.7)] to methanol is 85:15;

[0071] Condition ②: The volume ratio of [10mmol / L sodium pyrophosphate + 20mmol / L tetrabutylammonium bisulfate (pH8.2)] to methanol is 85:15;

[0072] Condition ③: The volume ratio of [10mmol / L sodium pyrophosphate + 20mmol / L tetrabutylammonium bisulfate (pH8.0)] to methanol is 85:15;

[0073] Flow rate: 1.0ml / min, detection wavelength: 215nm, column temperature: 30°C, injection volume: 20μl.

[0074] Take the system suitability solution 2 of Example 2 and carry out detection according to the above method. HPLC spectrum see Figure 3-5 , and the test results are shown in Table 5.

[00...

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Abstract

The invention provides a high performance liquid chromatography detection method for zoledronic acid and impurities of the zoledronic acid. The method includes the following chromatographic conditions: a stationary phase is a reversed phase chromatographic column with octylsilane bonded silica gel or octadecylsilane bonded silica as a filler; and a mobile phase is a mixture of a buffer solution and an organic solvent, wherein the buffer solution is a mixed solution of sodium pyrophosphate and tetrabutylammonium hydrogen sulfate having a concentration of 5-18 mmol / L or a mixture of sodium pyrophosphate and tetrahexyl ammonium hydrogen sulfate having a concentration of 5-18 mmol / L, a pH value of the buffer solution is 7.5-9.0, and the organic solvent is methanol or acetonitrile. The detection method provided by the invention can realize effective separation and detection of the zoledronic acid and the impurities of the zoledronic acid and solves the problems of compound retention and chromatographic peak trailing.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to a high-performance liquid chromatography detection method for zoledronic acid raw materials and impurities thereof. Background technique [0002] Zoledronic acid (Zoledronic Acid) is a third-generation bisphosphonic acid anti-osteoporosis drug, which is developed by Swiss company Norvartis for the treatment of hypercalcemia. It is mainly used clinically for the treatment of osteoporosis, hypercalcemia and Bone-related diseases caused by malignant tumors. The drug was first launched in Canada in October 2000. So far, the drug has been approved in more than 80 countries or regions including the European Union and the United States. In recent years, it has been found that it can induce the apoptosis of tumor cells, and it is expected to be directly used in the treatment of cancer. [0003] As a new class of bisphosphonic acid drugs, zoledronic acid has a chemical structure ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 张锋李丹刘音岑吴瑶余启波赵忠琼韩庆平王利春王晶翼
Owner SICHUAN KELUN PHARMA RES INST CO LTD
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