Ultrahigh pressure liquid phase detection method for prepared Chinese herb medicine
An ultra-high pressure liquid phase and detection method technology, applied in the ultra-high field, can solve the problems of difficult separation and long total time.
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Embodiment 1
[0140] Example 1. The quality detection method of Tongren Wuji Baifeng Pills (Darmi Pills, Tongrentang Pharmaceutical)
[0141] Instruments and reagents: Waters Acquity UPLC TM Ultra-high performance liquid chromatography-diode array detector (PDA), Waters Empower 2 data processing software system.
[0142] BüCHI rotary evaporator (Rotavapor R-114; Waterbath B-480); Lion Ding SHB-III circulating water multi-purpose vacuum pump (Zhengzhou Changcheng Technology Industry and Trade Co., Ltd.); KQ-250DE medical numerical control ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.); FW100 high-speed universal pulverizer (Tianjin Test Instrument Co., Ltd.). D-101 macroporous resin (Anhui Sanxing Resin Technology Co., Ltd.).
[0143] Methanol and ethanol are analytically pure reagents; UPLC uses acetonitrile (J.T.Baker Company) as chromatographically pure. Water is pure water, passed through Millipore 0.22μm filter membrane.
[0144] Paeoniflorin, Liquiritin, Ginsenoside R...
Embodiment 2
[0155] Example 2. The detection method of active ingredients in Wuji Baifeng Pills (Shuiwan, Huiren Pharmaceutical)
[0156] 1. Preparation of the solution of the test sample: Accurately weigh Wuji Baifeng Pills (water pill 6g), add methanol equivalent to about 8 times the amount of the test sample, dissolve, preferably ultrasonically treat for 20-40 minutes, filter, and recover the filtrate Concentrate the solvent to dryness, add about 50mL of water to the residue to dissolve, pass through a D101 macroporous resin adsorption column (the resin packed in the column is about 60g, the inner diameter is 2cm, and the length is 12cm), elute with about 300mL of water, discard the water, and then Elute with 50mL of ethanol with 25-35%wt, discard the eluate, continue to elute with 200mL of ethanol with 80%wt, collect the eluate, evaporate to dryness, dissolve the residue with methanol and transfer it to a 5mL volumetric flask, Add methanol to the scale, pass through a microporous membr...
Embodiment 3
[0161] Example 3. Detection method of active ingredients in other traditional Chinese medicine preparations containing two or more medicinal ingredients from Radix Paeoniae Alba, Ginseng, Danshen, Artemisia annua, Licorice, Rhizoma Chuanxiong, Angelica, Radix Astragali, and Rhizoma Cyperi
[0162] 1. Preparation of the test product solution: Accurately weigh 6 g of the test product (the test product contains Radix Paeoniae Alba, Radix Ginseng, Salvia miltiorrhiza), add methanol equivalent to about 8 times the amount of the test product, dissolve, filter, and the filtrate reclaims the solvent Concentrate to dryness, add about 50mL water to the residue to dissolve, pass through a D101 type macroporous resin adsorption column (about 60g of resin packed in the column), elute with about 300mL water, discard the water, and use 50mL ethanol with 25-35%wt Elution, discard the eluate, elute with 75% wt about 200mL ethanol, collect the eluate, evaporate to dryness, dissolve the residue w...
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