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Method for detecting contents of 1, 4, 7, 10-tetra-azacyclo dodecane (Cyclen) and derivatives thereof by using HPLC-ELSD

A technology of tetraaza heterocycle and dodecane, which can be used in measurement devices, instruments, scientific instruments, etc., can solve the problems of low sensitivity of differential detectors, and achieve the effects of good recovery rate, reduced damage, and avoidance of peak coincidence

Pending Publication Date: 2019-09-17
荆门医药工业技术研究院 +2
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Problems solved by technology

There is no report about the liquid phase content determination of Cyclen and its derivatives. Since Cyclen and its derivatives have no ultraviolet and fluorescence absorption, and the sensitivity of the differential detector is low, based on market demand, it is urgent to develop a method that is simple to operate, high in sensitivity, Rapid and accurate detection method to promote the research and development of Cyclen and its derivatives

Method used

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  • Method for detecting contents of 1, 4, 7, 10-tetra-azacyclo dodecane (Cyclen) and derivatives thereof by using HPLC-ELSD
  • Method for detecting contents of 1, 4, 7, 10-tetra-azacyclo dodecane (Cyclen) and derivatives thereof by using HPLC-ELSD
  • Method for detecting contents of 1, 4, 7, 10-tetra-azacyclo dodecane (Cyclen) and derivatives thereof by using HPLC-ELSD

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Embodiment Construction

[0025] The present invention is described in detail below in conjunction with specific embodiment

[0026] 1) Set detection conditions

[0027] HPLC conditions:

[0028] Chromatograph: Ultimate3000 High Performance Liquid Chromatography (Thermo Company)

[0029] Chromatographic column: ACE 4.6mm×250mm, particle size 5μm, Super C18 chromatographic column;

[0030] Mobile phase: mobile phase A is acetonitrile, mobile phase B is water;

[0031] Isocratic elution:

[0032] Acetonitrile: water = 50:50

[0033] Flow rate: 1.0mL / min;

[0034] ELSD conditions:

[0035] Using 2000ES ELSD detector (Aeltech company)

[0036] The temperature of the drift tube is 90°C, the nitrogen pressure is 0.4Mpa, and the gas flow rate (N 2 ) is 2.0L / min, Gain: 2, splitless mode

[0037] 2) Draw a standard curve

[0038] ① Draw the standard curve of Cyclen

[0039] 1. Weigh five groups of Cyclen standard products (TICIA Chemical Industry Development Co., Ltd., purity>99%), and dilute them in...

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Abstract

The invention discloses a method for detecting contents of 1, 4, 7, 10-tetra-azacyclo dodecane (Cyclen) and derivatives thereof by using HPLC-ELSD. The invention comprises the following steps: 1) arranging HPLC-ELSD conditions for detection: an HPLC condition: the ratio of flowing phase acetonitrile to water being 30-50: 50-70, and performing isocratic elution; an ELSD condition: the temperature of a drift tube being 75-105 DEG C, the pressure of N2 being 0.4-0.6 M pa, the flow rate of N2 being 1.6-2.2 L / min, the gain being 2-4, and carrying out a non-shunt mode; 2) drawing a standard curve; and 3) measuring the content of samples of the Cyclen and the derivatives thereof. The method for detecting contents of the Cyclen and the derivatives thereof by using HPLC-ELSD is good in specificity, repeatability, degree of precision and recovery rate.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for detecting the content of 1,4,7,10-tetraazacyclododecane and its derivatives by using HPLC-ELSD. Background technique [0002] The focus of research on macrocyclic amine compounds is 1,4,7,10-tetraazacyclododecane (Cyclen) and its derivatives. Due to their strong coordination ability with metal ions, they can complex with metal ions can be covalently attached to biomolecules. Cyclen and its derivatives are one of the commonly used intermediates of lanthanide-specific chelators, mainly compounds used in diagnostic and therapeutic drugs (eg, paramagnetic lanthanide chelates for MRI). Cyclen can also be used as an intermediate for N-alkylation to form a variety of compounds that can be used in molecular recognition and coordination chemistry. There is no report about the liquid phase content determination of Cyclen and its derivatives. Since Cyclen and its...

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Application Information

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IPC IPC(8): G01N30/02G01N30/38
CPCG01N30/02G01N30/38G01N2030/388
Inventor 彭佩罗磊胡亚丽张艳云
Owner 荆门医药工业技术研究院
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