Quality detection method of Chinese herb gentian
A detection method and technology of gentian can be used in pharmaceutical formulations, measuring devices, medical preparations containing active ingredients, etc., which can solve problems affecting the safety and effectiveness of clinical applications, and achieve high extraction efficiency and sample pretreatment process. simple effect
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Embodiment 1
[0014] (1) Preparation of test sample solution
[0015] Crush the traditional Chinese medicine gentian, pass through a 60-mesh sieve, weigh 50 mg of the crushed gentian, put it in a 50 ml conical flask, add 5 ml of methanol with a concentration of 50% by volume, and perform ultrasonic extraction once, 20 min / time, at a temperature of 20 ℃. Filter, combine the above extracts and concentrate to 1ml, dilute to 10ml with methanol, shake well, that is the test sample solution.
[0016] (2) Electrospray fingerprint of test sample
[0017] Take the test sample solution, dilute it 10 times with methanol, and analyze it by electrospray mass spectrometry. The experimental conditions of electrospray mass spectrometry are as follows: electrospray ionization source, spray voltage 3.5kV, capillary temperature 180°C, flow injection pump injection flow rate 2μl / min; scan range mass-to-charge ratio (m / z) 50-2000, using Spray mass spectrometry confirmed the species of secoiridoid glycosides....
Embodiment 2
[0022] (1) Preparation of test sample solution
[0023] Crush the traditional Chinese medicine gentian, pass through a 80-mesh sieve, weigh 200 mg of the crushed gentian, put it in a 50ml conical flask, add 20ml of methanol with a concentration of 100% by volume, and perform ultrasonic extraction for 3 times, 40min / time, at a temperature of 50°C . Filter, combine the above-mentioned extracts and concentrate to 2ml, dilute to 10ml with methanol, shake up, it is the test sample solution.
[0024] (2) Electrospray fingerprint of test sample
[0025] Take the test sample solution, dilute it 10 times with methanol, and analyze it by electrospray mass spectrometry. The experimental conditions of electrospray mass spectrometry are as follows: electrospray ionization source, spray voltage 5.5kV, capillary temperature 220°C, flow injection pump injection flow rate 8μl / min; scan range mass-to-charge ratio (m / z) 50-2000, using Spray mass spectrometry confirmed the species of secoirido...
Embodiment 3
[0030] (1) Preparation of test sample solution
[0031] Crush the traditional Chinese medicine gentian, pass through a 70-mesh sieve, weigh 150 mg of the crushed gentian, put it in a 50ml conical flask, add 15ml of methanol with a concentration of 75% by volume, perform ultrasonic extraction twice, 30min each time, and the ultrasonic extraction temperature is 35°C . Filtrate, combine the above extracts and concentrate to 1.5ml, dilute to 10ml with methanol, shake well, that is the test sample solution.
[0032] (2) Electrospray fingerprint of test sample
[0033]Take the test sample solution, dilute it 10 times with methanol, and analyze it by electrospray mass spectrometry. The experimental conditions of electrospray mass spectrometry are as follows: electrospray ionization source, spray voltage 4.5kV, capillary temperature 200°C, flow injection pump injection flow rate 6μl / min; scan range mass-to-charge ratio (m / z) 50-2000, using Spray mass spectrometry confirmed the spec...
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