Method for measuring flavone glycoside compounds in herba epimedii
A technology for determination of flavonoid glycosides in A. chinensis, which is applied in the field of determination of Epimedium, can solve the problems of weak anti-interference ability, inaccurate quantification, and difficulty in baseline separation, and achieves the effects of good accuracy, high sensitivity, and easy baseline separation.
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Embodiment 1
[0015] a. Weigh 0.5g of the Chinese herbal medicine Epimedium sample of 40 mesh sieves in a 100mL stoppered glass conical flask, add 50mL of 50% methanol-water solution (V / V), weigh, at normal temperature, under ultrasonic power Ultrasonic at 350W and ultrasonic frequency of 70KHz for 30min to make up the weight.
[0016] b. Take the supernatant and filter it with a 0.22um organic phase membrane to obtain the sample to be analyzed.
[0017] c. Analyze the obtained sample to be analyzed:
[0018] 1. Chromatographic conditions: Analytical column: Waters Acquity UPLC BEH C 18 (1.7μm, 2.1mm×50mm); mobile phase: phase A is 0.1% formic acid-water solution (V / V), phase B is acetonitrile solution; gradient condition: 0min, A: B (90%: 10%); 10min, A:B (80%:20%); 25min, A:B (70%:30%); 35min, A:B (50%:50%); 35.1min, A:B (0%:100 %); 39.9 min, A:B (0%:100%) 40.0 min, A:B (90%:10%). Flow rate: 0.25mL / min; column temperature 30°C.
[0019] 2. Mass spectrometry conditions: Quantitative a...
Embodiment 2
[0024] a. Take by weighing 0.4g of the Chinese herbal medicine Epimedium sample of 60 mesh sieves in a 100mL stoppered glass conical flask, add 40mL of 60% methanol-water solution (V / V), weigh, under normal temperature, at a rotating speed of 150r / Shake for 30 minutes at 2 min, let stand for 5 minutes, and make up the weight.
[0025] b. Take the supernatant and filter it with a 0.22um organic phase membrane to obtain the sample to be analyzed.
[0026] c. Analyze the obtained sample to be analyzed:
[0027] 1. Chromatographic conditions: Analytical column: Waters Acquity UPLC BEH C 18 (1.7μm, 2.1mm×50mm); mobile phase: phase A is 0.2% formic acid-water solution (V / V), phase B is acetonitrile solution; gradient condition: 0min, A: B (90%: 10%); 10min, A:B (80%:20%); 25min, A:B (70%:30%); 35min, A:B (50%:50%); 35.1min, A:B (0%:100 %); 39.9 min, A:B (0%:100%) 40.0 min, A:B (90%:10%). Flow rate: 0.25mL / min; column temperature 30°C.
[0028] 2. Mass spectrometry conditions: ...
Embodiment 3
[0030] a. Take by weighing 0.5 g of the Chinese herbal medicine Epimedium sample of 80 mesh sieves in a 100 mL glass conical flask with a stopper, add 20 mL of 70% methanol-water solution (V / V), weigh, and soak for 1.5 h at normal temperature, Make up weight.
[0031] b. Take the supernatant and filter it with a 0.22um organic phase membrane to obtain the sample to be analyzed.
[0032] c. Analyze the obtained sample to be analyzed:
[0033] 1. Chromatographic conditions: Analytical column: Waters Acquity UPLC BEH C 18 (1.7μm, 2.1mm×50mm); mobile phase: phase A is 0.3% formic acid-water solution (V / V), phase B is acetonitrile solution; gradient condition: 0min, A: B (90%: 10%); 10min, A:B (80%:20%); 25min, A:B (70%:30%); 35min, A:B (50%:50%); 35.1min, A:B (0%:100 %); 39.9 min, A:B (0%:100%) 40.0 min, A:B (90%:10%). Flow rate: 0.25mL / min; column temperature 30°C.
[0034] 2. Mass spectrometry conditions: Quantitative analysis was carried out in multiple reaction monitoring...
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