Rapid detection method of alkaloids in lotus seeds by electrospray extraction ionization mass spectrometry
A technology of alkaloid and electrospray, applied in the field of analysis
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Embodiment 1
[0030] 1 Experimental part
[0031] 1.1 Preparation of lotus seed alcohol solution:
[0032] 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.
[0033] 1.2 EESI-MS experimental parameters:
[0034] 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 3.0kV; the capillary temperature is 250 ℃; the ESI solvent is methanol; the atomizing gas is nitrogen (purity 99.999%), the pressure is 1.2MPa; the flow rate of EESI solvent and sample solution is 3 μL / min and 5 μ...
Embodiment 2
[0063] The electrospray extraction ionization mass spectrometry rapid detection method of alkaloids in lotus seeds comprises the following steps:
[0064] (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;
[0065](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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