Method for analyzing content of Abeta plaque imaging agent precursor AV-45-OTS through micellar electrokinetic chromatography

A technology of AV-45-OTS and plaque imaging agent, which is applied in the field of analytical chemistry, can solve the problems of difficult separation and polarity reduction of molecular structure, and achieve the effect of high separation efficiency, fast speed and reduced operating cost

Inactive Publication Date: 2015-11-04
JIANGSU INST OF NUCLEAR MEDICINE
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  • Abstract
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Problems solved by technology

Since the AV-45-OTS structure contains two protecting groups, BOC (tert-butoxycarbonyl protecting group) and OTS (p-toluenesulfonyl), the polarity of the molecular structure is greatly reduced, and ordinary high-performance liquid chromatography and other analysis methods are relatively Difficult to achieve ideal separation

Method used

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  • Method for analyzing content of Abeta plaque imaging agent precursor AV-45-OTS through micellar electrokinetic chromatography
  • Method for analyzing content of Abeta plaque imaging agent precursor AV-45-OTS through micellar electrokinetic chromatography
  • Method for analyzing content of Abeta plaque imaging agent precursor AV-45-OTS through micellar electrokinetic chromatography

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Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1, capillary selection and pretreatment:

[0028] Choose an uncoated 45cm×50μm quartz capillary column; first wash the new capillary column with methanol for 10min, distilled water for 5min, 1M NaOH solution for 30min, distilled water for 5min, and finally run buffer for 15min; Rinse with distilled water and running buffer for 2 min each.

Embodiment 2

[0029] Embodiment 2, the influence of sample solvent:

[0030] The sample AV-45-OTS is relatively insoluble. It cannot be completely dissolved in organic solvents such as methanol and acetonitrile. A large amount of such organic solvents must be added for complete dissolution. The peak inverted phenomenon was found in the sample injection, and repeated injections were very unstable, so it is not suitable as a sample solvent. Chromatographically pure tetrahydrofuran can completely dissolve the sample, and the dosage is not much. Moreover, tetrahydrofuran is aprotic and will not affect the electrostatic interaction with micelles, thus affecting the migration of solutes. Considering that the solvent in the sample solution must be miscible with the running buffer, we finally dissolved the sample in tetrahydrofuran and diluted it with borax buffer. That is, 1mg AV-45-OTS+0.5mL chromatographically pure tetrahydrofuran+1.5mL 25mmol / L borax-10mmol / L SDS is diluted and injected, and ...

Embodiment 3

[0031] Embodiment 3, chromatographic condition optimization:

[0032] 3.1 Selection of buffer system

[0033] From the partition mechanism of capillary electrokinetic chromatography, it can be known that the solute is partitioned between the micellar phase and the mobile phase, so changing the buffer system will affect the solute partition coefficient, and then affect the capacity factor and the retention value of the solute. The experiment first investigated the type of buffer, and used phosphate buffer (PBS), PBS-ammonium acetate system, and borax buffer system for experiments. The results showed that AV-45-OTS did not have a main peak in the PBS buffer system; In the ammonium system, there are obvious peaks, but the peak shape is very broad, and there is an inverted peak (see figure 1 ); using the borax buffer system, there was an obvious main peak, and the peak shape was sharper than that of the PBS-ammonium acetate system ( figure 2 ). Compared with the PBS system or ...

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Abstract

The invention discloses a method for analyzing the content of Abeta plaque imaging agent precursor AV-45-OTS through micellar electrokinetic chromatography and belongs to the technical field of analytical chemistry. The content of the AV-45-OTS can be easily and conveniently measured through a capillary electrophoresis method. An effective analysis means is provided for controlling the quality of a drug box, which is not reported in correlational research. 1 mg of the AV-45-OTS is precisely weighed and dissolved in 0.5 mL of chromatographic pure tetrahydrofuran and 1.5 ml of 25 mmol/L borax-10 mmol/L SDS solution, sample injection at the voltage of 10 kv is performed, the voltage is kept unchanged, the sample injection time is changed, linear regression is performed on the sample injection time at the peak area, the linear relation is good when the sample injection time is 8-16 s, the regression equation is y=112958x-525878, and the correlation coefficient r2 is equal to 0.9909. Compared with HPLC, the micellar electrokinetic chromatography has the main advantages that separation efficiency is high, the efficiency can be 500,000 theoretical plate number/m and is ten times that of the HPLC; the micellar electrokinetic chromatography has other advantages that speed is high, the quantity of samples in use is small, consumption of reagents is small, and running cost can be reduced.

Description

technical field [0001] The invention discloses a method for analyzing the content of AV-45-OTS, a precursor of Aβ plaque imaging agent, by micellar capillary electrokinetic chromatography, which belongs to the technical field of analytical chemistry. Background technique [0002] With the aging of China's population, Alzheimer's disease (AD) is increasing year by year, becoming the second most common neurological disease in the elderly after cerebrovascular disease, seriously affecting the quality of life of the elderly in their later years, and bringing great harm to society and families. a huge economic burden. The pathogenesis of AD is unknown and there is currently no cure. Only by making a correct diagnosis early and taking effective measures to delay the disease can the quality of life of the elderly be improved and social and family pressure reduced. At present, the aggregation of β-amyloid protein (Aβ) is considered clinically as the main pathological feature of AD...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 周杏琴毛师师彭颖张荣军张建康
Owner JIANGSU INST OF NUCLEAR MEDICINE
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