Construction method and detection method of uplc fingerprint of Angong Niuhuang Pills
A technology of Angong Niuhuang Pills and fingerprints, which is applied in the field of quality control of traditional Chinese medicine, can solve the problems of small number of characteristic peaks, long time, difficult quality evaluation of Angong Niuhuang Pills, etc., achieve high accuracy, short time, and improve quality detection efficiency effect
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Embodiment 1
[0038] This embodiment is a method for constructing UPLC fingerprints of Angong Niuhuang Pills.
[0039] 1. Materials
[0040] 1.1 Instrument
[0041] ACQUITY UPLC H-Class ultra-high performance liquid chromatography (Waters Shanghai Technology Co., Ltd.); Agilent G6500UPLC tandem quadrupole time-of-flight mass spectrometer (Agilent Technologies Co., Ltd.); Waters Xevo G2-Q-TOF (Waters Shanghai Technology Co., Ltd.) Co., Ltd.); BX8200HP Ultrasonic Apparatus (Shanghai Xinmiao Medical Instrument Manufacturing Co., Ltd.); Sartorius BP211D 1 / 100,000 Electronic Analytical Balance (Sartorius, Germany); Ultrapure Water System (Millpore, USA).
[0042] 2. Methods and results
[0043] 2.1 Fingerprint establishment
[0044] 2.1.1 Chromatographic conditions
[0045] Chromatographic column: Poroshell 120EC-C18 (2.1*100mm, 2.7μm); mobile phase: methanol (B)-volume concentration 0.1% formic acid water (A); elution gradient (volume fraction): 0-6min 10%-25% B, 6-22min25%-46%B, 22-24min ...
Embodiment 2
[0092] This embodiment is a detection method of Angong Niuhuang Pills, the steps are as follows:
[0093] 1. Chromatographic conditions
[0094] See item "2.1.1 Chromatographic conditions" in Example 1.
[0095] 2. Preparation of sample solution to be tested: Take Angong Niuhuang Pills to be tested (batch number: X02018), cut into pieces, take about 0.5g, accurately weigh it, put it in a 50mL conical flask with a stopper, and accurately add methanol with a volume concentration of 75% 25mL, packed tightly, weighed, mixed evenly, treated with ultrasonic (400W, 40kHZ) for 60min, allowed to cool, weighed again, supplemented the lost weight with methanol with a volume concentration of 75%, shaken well, let stand, the supernatant Filter through a microporous membrane (0.22 μm), and take the subsequent filtrate, that is, the obtained product.
[0096] 3. Determination: Precisely draw 2 μL of the sample solution to be tested, inject it into an ultra-high performance liquid chromatog...
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