Unlock instant, AI-driven research and patent intelligence for your innovation.

A pr-hplc method for simultaneously determining the content of five amino acids in dilong injection

A determination method, amino acid technology, applied in the field of instrument analysis, can solve problems such as complex operation, achieve strong specificity, simple and fast operation and analysis steps, and reduce the use of reagents

Inactive Publication Date: 2016-02-03
广东新峰药业股份有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although alanine, valine, lysine hydrochloride, isoleucine, and leucine have a good linear relationship within their respective concentration ranges, with an average recovery of 102.6~104.9% and an RSD of 0.3~0.9%, they need to use To the derivatizing agent for derivatization determination, the operation is complicated

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
  • A pr-hplc method for simultaneously determining the content of five amino acids in dilong injection
  • A pr-hplc method for simultaneously determining the content of five amino acids in dilong injection
  • A pr-hplc method for simultaneously determining the content of five amino acids in dilong injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 Dilong Injection Amino Acid Content Determination

[0023] Determination of the contents of five amino acids in Dilong injection, the five amino acids are alanine, valine, lysine hydrochloride, isoleucine, and leucine.

[0024] The measurement steps are:

[0025] S1. Chromatographic conditions: C18 reverse-phase chromatographic column, column temperature: 37°C, detection wavelength 248nm, flow rate 0.8ml / min gradient elution, mobile phase A is 0.7% trifluoroacetic acid aqueous solution of 5.0mmol / L heptafluorobutyric acid, The mobile phase B is 60% acetonitrile aqueous solution, and the gradient elution program is 0min100%A, 0.5min98.5%A, 10min90%A, 15min67%A, 20min20%A, 25min0%A;

[0026] S2. Preparation of reference substance solution: Accurately weigh 90.79 mg of alanine reference substance, 39.94 mg of valine reference substance, 32.53 mg of lysine hydrochloride reference substance, 30.87 mg of isoleucine reference substance, Leucine reference substan...

Embodiment 2

[0033] Embodiment 2 linear relationship investigation

[0034] Take the above-mentioned reference substance solution, accurately measure 1.0, 2.0, 4.0, 5.0, 6.0, 8.0, 10.0 μl respectively and inject into the high-performance liquid chromatograph, record the chromatogram, measure its peak area integral value, take the reference substance concentration as the abscissa, The corresponding peak area integral value is on the ordinate, and the linear regression calculation is performed on the reference substance concentration (injection volume) X with the peak area integral value Y, where the alanine regression equation is y=2921.3x-16.4, r=0.99978 (n =7), valine regression equation y=2598x+1.94, r=0.99998 (n=7), lysine hydrochloride regression equation y=2743.6x+0.87, r=0.99997 (n=7), isoleucine Regression equation y=2391.8x+1.6, r=0.99998 (n=7), leucine regression equation y=2406x-3.6, r=0.99997 (n=7). The results showed that alanine was in the range of 0.045395~0.453950μg, valine...

Embodiment 3

[0037] Embodiment 3 repeatability test

[0038] Take the same batch of Dilong injection (batch number 060703) to prepare 6 parts of the test solution according to the law, and accurately measure 5.0 μl of the sample for determination. The results are shown in Table 3. Alanine, valine, lysine hydrochloride, The RSDs of isoleucine and leucine content were 0.92%, 0.73%, 0.97%, 0.75%, 0.89%, respectively.

[0039] Table 3 Repeatability test results

[0040]

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
recovery rateaaaaaaaaaa
Login to View More

Abstract

The invention discloses a PR-HPLC (phase reversing-high performance liquid chromatography) determination method for simultaneously determining contents of five amino acids in earthworm injection. The method is characterized by comprising the following steps: preparing chromatographic conditions: a C18 or C8 phase reversing chromatographic column, column temperature: 37 DEG C, a detection wavelength: 248nm, gradient elution with flow rate of 0.8ml / min, a flowing phase A is 0.7% trifluoroacetic acid aqueous solution of 5.0mmol / L heptafluorobutyric acid, a flowing phase B is a 60% acetonitrile aqueous solution, and the flow rate of elution solution is as follows: 0 min 100%A, 0.5 min 98.5%A, 10min 90%A, 15min 67%A, 20min 20%A and 25min 0%A; preparing a reference solution and a test solution; and respectively measuring 10 microliters of reference solution and 10 microliters of test solution, respectively injecting the reference solution and the test solution into a phase reversing liquid chromatography, and carrying out the phase reversing liquid chromatographic determination and analysis. The determination method is simple and rapid in operation, and no derivating agent is needed; moreover, the stability is high, the repeatability is good, and the active ingredients and quality of the earthworm injection can be better controlled.

Description

technical field [0001] The invention relates to the technical field of instrumental analysis, in particular to a PR-HPLC method for simultaneously determining the contents of five amino acids in Dilong injection. Background technique [0002] Dilong Injection, relieves asthma and relieves cough. For cough and wheezing caused by bronchial asthma. [0003] In the early days, the content determination of Dilong injection consisted of three parts, namely nitrogen determination for total nitrogen, titration for amino nitrogen and thin layer chromatography for valine content. However, this determination method is not specific and heavy The realizability is not high, and the active ingredient and quality of Dilong injection cannot be controlled. [0004] Huang Lumin disclosed a method for establishing and determining the content of main amino acids in Dilong Injection in "Chinese Pharmacist", Volume 13, No. 11, 2010, "HPLC Determination of Main Amino Acid Contents in Dilong Injec...

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 & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 任宏李冠儒谢作君
Owner 广东新峰药业股份有限公司