Electrospray extraction ionization-mass spectrum (EESI-MS) rapid detection method for alkaloid in lotus seeds

A technology of alkaloid and electrospray, applied in the field of analysis

Active Publication Date: 2014-05-14
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the rapid analysis and identification of lotus alkaloids based on direct mass spectrometry has not been reported so far.

Method used

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  • Electrospray extraction ionization-mass spectrum (EESI-MS) rapid detection method for alkaloid in lotus seeds
  • Electrospray extraction ionization-mass spectrum (EESI-MS) rapid detection method for alkaloid in lotus seeds
  • Electrospray extraction ionization-mass spectrum (EESI-MS) rapid detection method for alkaloid in lotus seeds

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1 Experimental part

[0030] 1.1 Preparation of lotus seed alcohol solution:

[0031] In the first ten days of September 2012, the lotus seeds harvested in each year (2012, 2011, 2010, 2009) were crushed and passed through a 80-mesh sieve, and 0.01 g of the lotus seed powder was weighed, added to a 1.5 mL centrifuge tube, and 1 mL of 80 % ethanol solution, ultrasonically extracted for 10 min, and centrifuged at 4000 r / min for 5 min, the extracted supernatant was used as a sample for direct mass spectrometry detection, and each sample was tested 6 times in parallel.

[0032] 1.2 EESI-MS experimental parameters:

[0033] LTQ-MS works in the positive ion detection mode, and the scanning range of the mass spectrometer is m / z 50~1000; the ionization voltage is 3.0 kV; the capillary temperature is 250 ℃; the ESI solvent is methanol; the atomizing gas is nitrogen (purity 99.999%), the pressure is 1.2 MPa; the flow rate of EESI solvent and sample solution is 3 μL / min and 5...

Embodiment 2

[0062] The electrospray extraction ionization mass spectrometry rapid detection method of alkaloids in lotus seeds comprises the following steps:

[0063] (1) Sample treatment: Take lotus seeds, crush them, pass through an 80-mesh sieve, weigh 0.01 g of each lotus seed powder, add to a 1.5 mL centrifuge tube, add 1 mL of 80% ethanol solution, ultrasonically extract for 10 min, and centrifuge at 4000 r / min for 5 min. The extracted supernatant is used as a sample to be tested;

[0064](2) Preparation of standard products: Weigh 5 mg of liensinine, methyl liensinine, liensinine quaternary ammonium, nuciferine, and O-desmethylnuciferine reference substance, which are dried to constant weight, and use 80% methanol Dissolved, respectively prepared into a concentration of 1.00 mg / mL reference substance stock solution. Mix the stock solutions of each reference substance into a mixed standard loading sample, the concentrations are 0.03, 0.06, 0.12, 0.24, 0.48, 1.00 mg / mL, ready to use...

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Abstract

The invention relates to an electrospray extraction ionization-mass spectrum (EESI-MS) rapid detection method for alkaloid in lotus seeds, belongs to the technical field of analysis, and particularly relates to a rapid determination method for alkaloid in lotus seeds. The method comprises the following steps: processing a sample, processing a standard product, detecting by EESI-MS, drawing a standard curve, and calculating the concentration of alkaloid in a sample. The method provided by the invention is rapid and accurate without complex sample pretreatment, not only can be used for rapidly identifying the alkaloid in a complex matrix sample, but also can effectively differentiate lotus seed samples with different aging degrees by combining with chemometrics.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to the detection of lotus seed active substances. technical background [0002] lotus( Nelumbo nucifera Gaertn.) is a perennial aquatic herbaceous plant of Nymphaeaceae, widely distributed in tropical and subtropical regions. Lotus seed is the seed of lotus, which is rich in polysaccharides, phospholipids, alkaloids and flavonoids and other nutritional and health ingredients. [0003] Alkaloids are the main bioactive components of lotus, which can be detected in various parts of lotus. The traditional identification method of alkaloids is based on the chemical degradation method to identify the chemical structure of alkaloids. In recent years, modern analytical methods such as spectral analysis, mass spectrometry and nuclear magnetic analysis have been used to identify the structure of alkaloids. In recent years, great achievements have been made in the research on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64
Inventor 罗丽萍陈焕文戴喜末方小伟
Owner NANCHANG UNIV
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