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Method for determining pinanediol content in bortezomib by adopting high performance liquid chromatography

A high-performance liquid chromatography and pinanediol technology, which is applied in the field of high-performance liquid chromatography for determining the content of pinanediol in bortezomib, can solve the problems of inability to detect, low sensitivity, and inability to reproduce the method, and achieves precise The effect of good degree, high sensitivity and strong specificity

Active Publication Date: 2022-03-01
CHONGQING MEDICAL & PHARMA COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Specifically, pinanediol has two configurations (R-type and S-type), and the boiling point of this type of compound is high (the boiling point of S-type is 239.9°C), and headspace detection leads to low sensitivity; Boric acid damages the chromatographic column, and the method cannot be reproduced; derivatized with trifluoroacetic acid, the derivatives are 3 different compounds, and the derivatization ratio is unstable; it is difficult to meet the detection requirements with GC
Such compounds have no ultraviolet absorption, so UV detectors cannot be used. Evaporative photodetectors and differential refractive index detectors are correspondingly low for such compounds, and the sensitivity cannot meet the detection requirements. Common HPLC cannot detect them. The literature has not yet found pinene in bortezomib. The detection method of alkanediol, that is, the analysis and detection of pinanediol in bortezomib is still blank at present, so how to quickly and accurately separate and determine the content of pinanediol in bortezomib has become an urgent problem to be solved at present

Method used

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  • Method for determining pinanediol content in bortezomib by adopting high performance liquid chromatography
  • Method for determining pinanediol content in bortezomib by adopting high performance liquid chromatography
  • Method for determining pinanediol content in bortezomib by adopting high performance liquid chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The selection of embodiment 1 chromatographic conditions

[0036] 1.1 Selection of wavelength

[0037] Pinanediol derivative solution: weigh about 10 mg of pinanediol derivative, put it in a 10ml measuring bottle, add acetonitrile as a diluent to dissolve, dilute to the mark, shake well, and you get it.

[0038] Take the pinanediol derivative solution as the test sample, use acetonitrile as the blank calibration solution, and scan at 190-400nm according to the ultraviolet-visible spectrophotometry (Chinese Pharmacopoeia 2020 edition). The results showed that the test solution had a plateau absorption peak at 270nm, so 265-275nm was determined as the detection wavelength.

[0039] 1.2 Durability test of the method

[0040] In this test, the chromatographic method of this test is screened by adjusting the mobile phase ratio, flow rate, column temperature, etc. The specific scheme is shown in Table 1 below.

[0041] Screening scheme for the method in Table 1

[0042] ...

Embodiment 2

[0050] The stability of embodiment 2 solution

[0051] Chromatographic conditions: the same as in Example 1, Scheme 1.

[0052] Pinanediol derivative solution: Accurately weigh 15mg of pinanediol derivative, put it in a 50ml measuring bottle, add acetonitrile to dissolve and dilute to the mark, shake well, and you get it;

[0053] Pinanediol derivative reference solution: accurately measure 1ml of the pinanediol derivative solution, place it in a 100ml measuring bottle, dilute to the mark with acetonitrile, shake well, and get it;

[0054]Need testing solution: prepare by the same method of 100% concentration level need testing solution in embodiment 1;

[0055] Reference substance solution:

[0056] At 0 hour, 4 hours, 12 hours, 24 hours, and 48 hours, 10 μl of the test solution and control solution were precisely measured, and the chromatograms at different time points were recorded. The results are shown in Table 3 below.

[0057] Table 3 solution stability result

[00...

Embodiment 3

[0060] The making of embodiment 3 standard curve

[0061] Chromatographic conditions: the same as in Example 1, scheme 1.

[0062] Solution preparation:

[0063] Linear stock solution: Accurately weigh 15mg of pinanediol derivatives, place in a 50ml measuring bottle, add acetonitrile to dissolve and dilute to the mark, shake well, and obtain;

[0064] Standard curve solution: dilute the linear stock solution with acetonitrile to prepare solutions of pinanediol derivatives with different concentrations, as shown in Table 4 below.

[0065] The preparation of table 4 standard curve solution

[0066] Measure the volume of linear stock solution (ml) Measuring bottle (ml) Concentration of pinanediol derivatives (μg / ml) 1 (pinanediol reference substance solution) 10 0.3 1 200 1.5 1 100 3 1 50 6 1 25 12

[0067] The results show that the pinanediol derivatives are in the range of 0.2976 μg / ml to 11.8638 μg / ml, the linear equation is ...

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Abstract

The invention provides a method for determining the pinanediol content in bortezomib by adopting a high performance liquid chromatography, and the chromatographic conditions in the method are as follows: octadecyl bonded silica gel is used as a chromatographic column of a filler, acetonitrile-0. 1% phosphoric acid water with the volume ratio of 70: 30-85: 15 is used as a mobile phase, the flow velocity is 0.8-1.2 ml / min, the detection wavelength is 265-275 nm, the sample size is 5-100 microliters, the column temperature is 20-30 DEG C, and the detection time is 2-4 hours. A sample solution is prepared by adopting a derivatization reaction taking bortezomib as a derivatization reagent. According to the method, bortezomib is used as a derivatization reagent, pinane diol is prepared into the pinane diol derivative, the content of pinane diol in bortezomib is quantitatively measured by measuring the pinane diol derivative, and the method is high in specificity, good in precision and high in accuracy and can be used for rapidly and accurately measuring the content of pinane diol.

Description

technical field [0001] The invention relates to the technical field of medical detection, in particular to a method for measuring the content of pinanediol in bortezomib by high performance liquid chromatography. Background technique [0002] Bortezomib (BTZM) is a synthetic alanine-based boronic acid derivative, which is used in the treatment of multiple myeloma. Clinical data show that bortezomib has obvious curative effects on cervical cancer, lymphoma, stem cell tumor, etc. , so the drug has gradually become an important anti-tumor drug and has become a hot spot in domestic generic drug research. [0003] [0004] In recent years, the requirements for isomers in drugs have become more and more stringent, not just the limit requirements, but the accurate determination of their content. The final step in the synthetic route of bortezomib is generally to remove the pinanediol protecting group, so detecting the residual pinanediol in bortezomib becomes an important conte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027Y02A50/30
Inventor 马潋邱妍川韦丽佳
Owner CHONGQING MEDICAL & PHARMA COLLEGE