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Detection method of minodronic acid by using high performance liquid chromatography

A high-performance liquid chromatography and chromatographic column technology, which is applied in the field of high-performance liquid chromatography for detecting minodronic acid, can solve the problems of less detection of impurity peaks, no strong chromophore, poor separation of impurities, and the like, To achieve the effect of good system applicability and good tailing factor

Inactive Publication Date: 2014-08-13
Yung Shin Pharm Ind (Kunshan) Co Ltd
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It began to be used in the treatment of OP in the mid-1970s, but long-term use will prevent normal bone tissue calcification and increase the incidence of fractures
③Most bisphosphonates do not have strong chromophores, so there is no universal method for chromatographic analysis of such drugs
[0009] Patent US005480875A and literature (Wu Fangning, Determination of Minodronic Acid in Minodronic Acid Tablets by High Performance Liquid Chromatography [J], Modern Drugs and Clinics, 2011, (26) 1:66-67) disclosed minodronic acid drug The liquid chromatographic conditions of the high-performance liquid phase detection method, however, this detection condition is not suitable for this substance, the impurity separation degree is not good, the number of impurity peaks is detected less, the number of theoretical plates is low, and the quality of minodronic acid cannot be accurately evaluated. Lack of authenticity and accuracy of data

Method used

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  • Detection method of minodronic acid by using high performance liquid chromatography
  • Detection method of minodronic acid by using high performance liquid chromatography
  • Detection method of minodronic acid by using high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: The method for detecting minodronic acid using high performance liquid chromatography

[0030]Get 10 minodronic acid tablets, grind into powder, make test sample;

[0031] Take 1L of deionized water, add 0.02mol (5.32g) sodium pyrophosphate, 0.322g tetrabutylammonium bromide, after dissolving, add phosphoric acid to adjust the pH to 8.0, take 950ml of the above solution, add 50ml of methanol, and prepare the mobile phase;

[0032] Get need testing sample 150mg, be diluted to 10ml with described mobile phase, obtain need testing sample solution;

[0033] Get described need testing solution 1ml, dilute to dilute 100ml with mobile phase and obtain contrast solution;

[0034] Adjust the flow rate of the high-performance liquid chromatograph to 1.0ml / min, the detection wavelength to 218nm, take 20 μl of the control solution and inject it into the high-performance liquid chromatograph, and adjust the detection sensitivity so that the peak height of the main com...

Embodiment 2

[0037] Embodiment 2: investigation of mobile phase aqueous solution and methanol ratio

[0038] Using the aqueous solution that contains 0.02mol / L sodium pyrophosphate and 0.322g / L tetrabutylammonium bromide prepared according to embodiment 1, the volume ratio of aqueous solution and methanol is respectively 90:10, 95:5, 100:0 Three mobile phases. All the other conditions are identical with embodiment 1, and the high performance liquid chromatogram of gained is shown in figure 2 , where A, B, and C are the chromatograms of the three mobile phases respectively. The resolution, retention time of main peak and number of impurity peaks of different mobile phases are shown in Table 1.

[0039] Table 1 The resolution, main peak retention time and impurity peak quantity of different mobile phase ratios

[0040]

[0041] It can be seen that with the decrease of the organic phase in the mobile phase, the retention time of the main peak is extended, and the separation degree of t...

Embodiment 3

[0042] Embodiment 3: the investigation of sodium pyrophosphate concentration

[0043] Take 1L of deionized water, add 0.02mol (5.32g), 0.03mol (7.98g) and 0.04mol (10.64g) sodium pyrophosphate, 0.322g tetrabutylammonium bromide, add phosphoric acid after dissolving to adjust the pH to 8.0, take 950ml, mixed with 50ml methanol to prepare three mobile phases respectively. All the other conditions are the same as in Example 1. The resulting high performance liquid chromatography see image 3 , where A, B, and C are the chromatograms at concentrations of 0.02, 0.03, and 0.04mol / L sodium pyrophosphate, respectively. The resolution, retention time of main peak and number of impurity peaks of different mobile phases are shown in Table 2.

[0044] Table 2 The degree of separation and the retention time of the main peak and the number of impurity peaks with different concentrations of sodium pyrophosphate

[0045]

[0046]

[0047] As the concentration of sodium pyrophosphate...

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Abstract

The invention discloses a detection method of minodronic acid by using high performance liquid chromatography. The method includes following chromatogram conditions: employing a mixed solution, which is composed of methanol and an aqueous solution containing sodium acid pyrophosphate and tetra butyl ammonium bromide, as a mobile phase with a volume ratio of the aqueous solution to the methanol ranging from 90:10 to 100:0, wherein the pH value of the aqueous solution is 7.0-8.0, the concentration of the sodium acid pyrophosphate is 0.02-0.04 mol / L and the concentration of the tetra butyl ammonium bromide is 0.272-0.322 g / L; employing octade-cylsilane (ODS) as a packing material, setting a flow velocity of a high performance liquid chromatography instrument to be 0.8-1.2 ml / min, a detection wavelength to be 218-282 nm and a sample size being 5-50 [mu]l. With the detection method, separation degrees, between a main peak and a neighboring impurity peak, in both a to-be-tested sample and a raw material are more than 1.5; and main peak column efficiencies in both the to-be-tested sample and the raw material are more than 3000. The detection method is good in trailing factor and system applicability.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to a method for detecting minodronic acid by using high performance liquid chromatography. Background technique [0002] Osteoporosis (OP) is a multifactorial systemic bone disease characterized by decreased bone strength and increased fracture risk due to increased bone fragility. Bone strength depends primarily on two factors: bone mineral density and bone quality. Factors affecting bone quality include bone microarchitecture, bone turnover, damage accumulation (such as microfractures), and bone mineralization status. Decreased bone strength makes bones prone to fracture when subjected to external forces. With the extension of human life span, aging is a new problem affecting human health. Osteoporosis and the fractures it causes rank seventh among current common diseases, seriously threatening the health of middle-aged and elderly people, and becoming a global public he...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 刘佳王莉林维政
Owner Yung Shin Pharm Ind (Kunshan) Co Ltd
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