Quality detection method of trientine hydrochloride

A quality testing method and technology of trientine hydrochloride, applied in the field of quality testing of trientine hydrochloride, can solve the problems of special requirements for testing equipment, inability to analyze impurities, and high levels of diethylenetriamine, and achieve increased detection and separation capabilities, Save analysis time, simple operation effect

Inactive Publication Date: 2019-01-18
凯默斯医药科技上海有限公司
View PDF4 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method still has big defects. On the one hand, this method can only separate the above-mentioned three specific impurities, but cannot analyze other possible impurities, which is also a fatal flaw of the method; on the other hand, although the method The sensitivity of diethylenetriamine has been improved, but the detection limit of diethylenetriamine is still as high as 27.5ng, and its operation is complicated, time-consuming and laborious, and has special requirements for detection equipment, so it is not suitable for application and promotion in the pharmaceutical industry

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Quality detection method of trientine hydrochloride
  • Quality detection method of trientine hydrochloride
  • Quality detection method of trientine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The quality detection method of embodiment 1 trientine hydrochloride of the present invention

[0033] Agilent 7890A gas chromatograph was used.

[0034] Take about 50mg of this product, weigh it accurately, add 0.3mL 3mol / L ammonia solution, add water to quantitatively dilute to 10mL, shake well, and use it as the sample solution; An appropriate amount of oxazine, tris(2-aminoethyl)amine, N-[2-(1-piperazinyl)ethyl]-1,2-ethylenediamine reference substance, dissolved in water and quantitatively diluted to make each 1mL The mixed solution containing 50 μg of each impurity is used as the impurity positioning solution; the CP-Volamine (0.53mm×30m×0.5μm) quartz capillary column is used as the chromatographic column, maintained at 190°C for 40 minutes; the column flow rate is 1.0mL / min; the detector is hydrogen Flame ionization detector (FID), the detector temperature is 350°C; the inlet temperature is 300°C, and the split ratio is 5:1. Precisely measure 0.1 μL each of the ...

Embodiment 2

[0038] The quality detection method of embodiment 2 trientine hydrochloride of the present invention

[0039] Agilent 7890A gas chromatograph was used.

[0040]Take about 100mg of this product, weigh it accurately, add 1.5mL 1mol / L ammonia solution, add water to quantitatively dilute to 10mL, shake well, and use it as the sample solution; An appropriate amount of oxazine, tris(2-aminoethyl)amine, N-[2-(1-piperazinyl)ethyl]-1,2-ethylenediamine reference substance, dissolved in water and quantitatively diluted to make each 1mL The mixed solution containing 30 μg of each impurity was used as the impurity positioning solution; the CP-Volamine (0.32mm×30m×3μm) quartz capillary column was used as the chromatographic column, the initial temperature was 50°C, maintained for 5min, and then the temperature was raised to 200°C at a rate of 20°C / min. ℃, maintained for 20min; the column flow rate was 1.5mL / min; the detector was a hydrogen flame ionization detector (FID), and the detector ...

Embodiment 3

[0044] The quality detection method of embodiment 3 trientine hydrochloride of the present invention

[0045] Agilent 7890A gas chromatograph was used.

[0046] Take about 200mg of this product, weigh it accurately, add 0.5mL 10mol / L potassium hydroxide solution, add water-ethanol (70:30) to quantitatively dilute to 10mL, shake well, and use it as the sample solution; An appropriate amount of diethylenetriamine, aminoethylpiperazine, tris(2-aminoethyl)amine, N-[2-(1-piperazinyl)ethyl]-1,2-ethylenediamine reference substance, add water -Ethanol (70:30) was dissolved and quantitatively diluted to make a mixed solution containing 20 μg of each impurity per 1 mL as an impurity positioning solution; a CP-Volamine (0.32mm×30m×3 μm) quartz capillary column was used as a chromatographic column, and the initial temperature 100°C, maintained for 20min, then raised to 220°C at a rate of 10°C / min, and maintained for 10min; the column flow rate was 2.0mL / min; the detector was a hydrogen f...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
concentrationaaaaaaaaaa
melting pointaaaaaaaaaa
recovery rateaaaaaaaaaa
Login to View More

Abstract

The invention provides a quality detection method of trientine hydrochloride. The method detects impurities such as ethylenediamine, diethylenetriamine, aminoethylpiperazine, tris(2-aminoethyl)amine and N-[2-(1-piperazinyl)ethyl]-1,2-ethanediamine in trientine hydrochloride by a gas chromatography. The detection method of the invention can quantitatively analyze and detect known impurities such asethylenediamine, diethylenetriamine, aminoethylpiperazine, tris(2-aminoethyl)amine and N-[2-(1-piperazinyl)ethyl]-1,2-ethanediamine, and has strong specificity, high sensitivity and good reproducibility. The method can measure the related substances of the trientine hydrochloride, and can quantitatively measure three kinds of known impurities, diethylenetriamine, methane and ethylene, in an amount of 0.05% or less, and can increase the detection and separation ability for other unknown impurities, therefore, the technical bias that the boiling point of trientine hydrochloride is high and thegas phase detection cannot be performed is overcome. The quality detection method of the trientine hydrochloride is simple in operation, thereby effectively saving the analysis time, and improving thework efficiency.

Description

technical field [0001] The invention relates to a quality detection method of trientine hydrochloride. It belongs to the field of drug testing. Background technique [0002] Hepatolenticular degeneration, also known as Wilson's disease, is an autosomal recessive inherited disorder of copper metabolism, which is caused by mutations in the ATP7B gene. Clinically, the disease has liver type, brain type, mixed type and asymptomatic type. Renal impairment and corneal pigment rings. [0003] The worldwide prevalence of hepatolenticular degeneration is 3 / 100,000, of which gene carriers account for 1 / 90. The treatment plan for this type of disease follows the principles of early diagnosis and early treatment. However, before the mutated gene is completely corrected, the purpose of drug treatment can only be to promote the excretion of copper in the body and reduce the absorption of copper, which requires a long-term Therefore, patients need to receive lifelong drug treatment, in...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & AuthorityApplications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor董竞傅霖陈刚
Owner凯默斯医药科技上海有限公司