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Super fast liquid phase chromatography-tandem mass spectrometric method for determining hydroxypropyl-beta-cyclodextrin

A technology of liquid chromatography and tandem mass spectrometry, which is applied in the direction of measuring devices, instruments, and material analysis through electromagnetic means, can solve problems that have not been reported in the literature, and achieve fast analysis speed, simple operation, and good reproducibility.

Inactive Publication Date: 2011-11-23
贾正平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many reports on the characteristics and applications of HP-β-CD, such as the patent No. ZL02116766.4 in the Chinese patent database from 1984 to 2009 "Complexes of organic drugs and beta-cyclodextrin derivatives and their Preparation Method", Application No. 02149146.1 "Anticancer Drug Paclitaxel Self-emulsifying Solid Nanoparticles - Preparation Method of Paclitaxel for Injection", Patent No. ZL03825141.8 "Aqueous Filling Composition Stabilized with Derivative Cyclodextrin capsules”, etc., but there are no literature reports on the chromatography and mass spectrometry methodology for quantitative research

Method used

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  • Super fast liquid phase chromatography-tandem mass spectrometric method for determining hydroxypropyl-beta-cyclodextrin
  • Super fast liquid phase chromatography-tandem mass spectrometric method for determining hydroxypropyl-beta-cyclodextrin
  • Super fast liquid phase chromatography-tandem mass spectrometric method for determining hydroxypropyl-beta-cyclodextrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]Embodiment 1 measures the content of HP-β-CD in the preparation with ultra-fast liquid chromatography (UFLC)-tandem mass spectrometry (MS / MS), comprises the following steps:

[0043] (1) Preparation of HP-β-CD standard curve solution: Accurately weigh 0.0050 g of HP-β-CD standard product produced by NIHON SHOKUHIN Company in a 10ml volumetric flask, and use methanol- Water mobile phase to volume, shake well to get 500μg / ml HP-β-CD standard solution as stock solution; draw 200μl of stock solution into another 10ml volumetric flask, mobile phase to volume, shake well to get 10μg / ml HP-β-CD standard solution.

[0044] Take 500 μL, 10 μg / ml HP-β-CD standard solution in a 3ml centrifuge tube, add 1500 μL of mobile phase, put it into a vortex mixer (Jincheng Teaching Instrument Factory, Jintan City) and vortex to mix to obtain 2500ng / ml solution; take 800μL, 2500ng / ml solution in a 1.5ml centrifuge tube, add 200μL of mobile phase, put it into a vortex mixer and vortex to mix,...

Embodiment 2

[0050] Embodiment 2 measures the content of HP-β-CD in urine with ultrafast liquid chromatography (UFLC)-tandem mass spectrometry (MS / MS) to be 4.5mg / ml, and obtain chromatogram Figure 6 .

[0051] The preparation of HP-β-CD standard curve solution, HP-β-CD QC solution and liquid chromatography-tandem mass spectrometry analysis are the same as in Example 1.

[0052] Urine was used as the sample, and the processing method was as follows: use a pipette gun to accurately absorb the urine of the subject, add ethylenediaminetetraacetic acid (EDTA) at a volume of 1:1 to 1:2 of the urine, and put it in a vortex mixer. After vortex mixing in the homogenizer, add ammonia water with a urine volume of 1:50 to 1:55, vortex and mix to obtain a mixed solution, and then add methanol with a volume ratio of 1:1 to 9:1 to the mixed solution Water mobile phase, vortex and mix for 2 minutes, then put it into a high-speed centrifuge and centrifuge at a speed of 5000r / min for 5 minutes, use a pip...

Embodiment 3

[0053] Embodiment 3 is used to measure the ultra-fast liquid chromatography-tandem mass spectrometry of HP-β-CD, wherein the preparation of HP-β-CD standard curve solution, HP-β-CD QC solution and liquid chromatography-tandem mass spectrometry analysis all With embodiment 1.

[0054] The processing of the sample is the same as in Example 1 or Example 2.

[0055] The mobile phase is methanol-ammonium acetate with a volume ratio of 2:1-4:1; wherein the concentration of ammonium acetate is 1-10 mM.

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Abstract

The invention relates to a super fast liquid phase chromatography-tandem mass spectrometric method for determining hydroxypropyl-beta-cyclodextrin. The method comprises the following steps: (1) preparing hydroxypropyl-beta-cyclodextrin standard curve solution; (2) preparing hydroxypropyl-beta-cyclodextrin quality control solution; (3) treating a sample; and (4) performing liquid phase chromatography-tandem mass spectrometric analysis on the standard curve solution and the quality control solution respectively, and establishing a method for determining the hydroxypropyl-beta-cyclodextrin in the sample solution. The method has simple operation and good reproducibility, and can quantitatively analyze HP-beta-CD.

Description

technical field [0001] The invention relates to a mass spectrometry method in the field of analysis method application research, in particular to an ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS / MS) method for measuring hydroxypropyl-β-cyclodextrin. Background technique [0002] Hydroxypropyl-beta-cyclodextrin (Hydroxypropyl-beta-cyclodextrin; HP-β-CD) is a hydroxyalkylated derivative of β-cyclodextrin. , One of the β-CD derivatives with more thorough application research. HP-β-CD not only has excellent enveloping effect on many compounds like β-CD, can improve the stability of the enveloped substances, but also has high water solubility and improves the release of enveloped drugs in vivo Speed ​​and bioavailability, therefore, HP-β-CD has a wider range of applications because of its special and excellent characteristics, and has been widely used in medicine. Because the water solubility of HP-β-CD is greater than 50%, good fluidity, low hemolytic activ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/00G01N30/02G01N27/62
Inventor 贾正平王荣谢华张娟红
Owner 贾正平
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