Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Gas chromatographic-mass spectrometric detection method of higenamine in multiple matrix samples

A technique for higenamine and mass spectrometry detection, applied in the field of book chemical analysis, can solve the problems such as the detection limit does not meet the ideal requirements, there is no analysis and research on Chinese patent medicines, and it does not have universal applicability, etc., and the extraction method is easy to operate. , the effect of improving sensitivity and accuracy, and low operating cost

Active Publication Date: 2019-03-26
HANDAN COLLEGE
View PDF4 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the LC-MS method has high sensitivity and low detection limit, it is expensive and does not have universal applicability; when LC detects higenamine enantiomers, a derivatized method is used, but the detection limit does not reach the ideal Require
The sample matrices reported in the literature are mainly plasma, urine, Chinese herbal medicine and dietary supplements, etc. There is no analysis and research on Chinese patent medicines

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
  • Gas chromatographic-mass spectrometric detection method of higenamine in multiple matrix samples
  • Gas chromatographic-mass spectrometric detection method of higenamine in multiple matrix samples
  • Gas chromatographic-mass spectrometric detection method of higenamine in multiple matrix samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 sample: blood plasma

[0034] After the plasma sample was thawed, the protein was precipitated with acetonitrile. The volume ratio of plasma to sample was 1:3. After precipitation, the supernatant was taken as the sample solution. Use PEP-2 (200mg / 6mL) solid-phase extraction column for extraction, first use 5mL methanol and 5mL water to activate the solid-phase extraction (SPE) column. Take 1mL sample solution for solid phase extraction, then rinse with 1mL 30% (V) methanol aqueous solution, and finally elute with 2mL 5% (V) formic acid methanol solution, and dry the eluent slowly with nitrogen flow at 70°C. Add 100 μL of heptafluorobutyric anhydride to the dried residue and derivatize at 70°C for 45 min. The derivatized sample solution is detected by gas chromatography-mass spectrometry, and the chromatogram is shown in figure 1 . figure 1 The curves in the middle are the curves of the blank plasma sample and the plasma sample after adding the standard sam...

Embodiment 2

[0035] Example 2: Sample: Urine

[0036]After the urine sample was thawed, the protein was precipitated with acetonitrile. The volume ratio of urine to sample was 1:3. After precipitation, the supernatant was taken as the sample solution. Take the supernatant as the sample solution. Use PEP-2 (200mg / 6mL) solid-phase extraction column for extraction, first use 5mL methanol and 5mL water to activate the solid-phase extraction (SPE) column. Take 1mL sample solution for solid phase extraction, then rinse with 1mL 30% (V) methanol aqueous solution, and finally use 2mL 5% (V) formic acid methanol solution for elution, and dry the eluent slowly with nitrogen flow at 70°C . Add 100 μL of heptafluorobutyric anhydride to the dried residue and derivatize at 70°C for 45 min. The derivatized sample solution is detected by gas chromatography-mass spectrometry, and the chromatogram is shown in figure 2 . figure 2 The middle curves are the blank urine sample and the urine sample after ...

Embodiment 3

[0037] Embodiment 3: sample solution preparation Chinese patent medicine

[0038] Take 50 μL of the solution and dilute it with water to 1 mL. Use PEP-2 (200mg / 6mL) solid-phase extraction column for extraction, first use 5mL methanol and 5mL water to activate the solid-phase extraction (SPE) column. Take 1mL sample solution for solid phase extraction, then rinse with 1mL 30% (V) methanol aqueous solution, and finally use 2mL 5% (V) formic acid methanol solution for elution, and dry the eluent slowly with nitrogen flow at 70°C . Add 100 μL of heptafluorobutyric anhydride to the dried residue and derivatize at 70°C for 45 min. The derivatized sample solution is detected by gas chromatography-mass spectrometry, and the chromatogram is shown in image 3 . image 3 The curves in the middle are the Chinese patent medicine samples in the blank solution and the Chinese patent medicine samples in the solution after adding the standard sample (25ng / mL). After being processed by the...

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
linear rangeaaaaaaaaaa
Login to View More

Abstract

The invention relates to a gas chromatographic-mass spectrometric detection method of higenamine in multiple matrix samples. The method comprises the following detection steps of (1), preparation of asample solution obtaining a higenamine extracting liquid sample solution from a solid sample through ultrasonic extraction, and directly using a solution sample as a sample solution; (2), solid phaseextraction: activating a solid phase extraction column by using methanol and water: taking and putting 1 mL of the sample solution into the solid phase extraction column, leaching by using a methanolaqueous solution, finally carrying out elution by using a formic acid-methanol solution, and slowly blow-drying eluent at 70 DEG C by using a nitrogen flow; (3), a derivation reaction: adding 50 muLto 150 muL of heptafluorobutyric anhydride into a residue, and deriving for 5 min to 60 min at 40 DEG C to 90 DEG C, so that a derived sample solution is made; and (4), gas chromatographic-mass spectrometric detection: subjecting the derived sample solution to gas chromatographic separation-mass spectrometric detection. According to the method, the ultrasonic extraction, the solid phase extractionand the deriving reaction are carried out on a sample; the preparation process of the sample is optimized; the higenamine in a drug can be effectively detected; and the detection sensitivity and accuracy are improved.

Description

technical field [0001] The technical field of chemical analysis of the present invention relates to a doping agent detection method, in particular to a gas chromatography-mass spectrometry detection method for higenamine in various matrix samples. Background technique [0002] Higenamine can stimulate β-adrenergic receptors, and through anti-platelet aggregation, inhibiting iNOS and up-regulating the expression of HO~1, it can have a positive and timely effect on the cardiovascular system. Therefore, higenamine is also used as a new type of Myocardial Stress Test Drugs. In January 2017, WADA included higenamine in group S3 (β2-receptor agonists) of the banned list. Higenamine is widely distributed in plants, including Nandina genus, Aconitum genus, Asarum genus, Sorrelia genus, Anemone genus and Nelumbo genus, etc. Athletes’ daily diet, nutritional supplements, and medication may contain Higendaline, which caused accidental ingestion by athletes. Relevant documents in Chi...

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 Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/7206
Inventor 王博王晓丽张萍萍连靠奇
Owner HANDAN COLLEGE
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com