Traditional Chinese medicine believes that sperm and blood are homologous, blood deficiency is also insufficient, intestinal fluid deficiency is easy to cause constipation. Angelica sinensis can moisten intestines and relieve constipation, often combined with semen seed, bitter almond and rhubarb to treat blood deficiency and constipation; and Fangfeng Tongshengsan, composed of Fangfeng Tongshengsan, Chuanxiong, Shaoyao, rhubarb, mint leaf and ephedra, can relieve heat and relieve constipation. Angelica Film,Angelica Acutiloba Root Extract,Angelica Keiskei Extract,Angelica Extractive Lixian Spring Pharmaceutical Co., Ltd. , https://www.lxctyy.com
Determination of mustard content by high performance liquid chromatography
Determination of mustard content by high performance liquid chromatography
The content was determined by high performance liquid chromatography (Appendix VI D).
Chromatographic conditions and system suitability test using octadecylsilane bonded silica as a filler; acetonitrile-0.08mol / L potassium dihydrogen phosphate (10:90) as mobile phase; detection wavelength is 326nm; theoretical plate number according to mustard The base peak should be calculated no less than 3,000.
Preparation of the reference solution The appropriate amount of the sinapine thiocyanate reference substance is accurately weighed and dissolved in a mobile phase to prepare a solution containing 0.2 mg per 1 ml.
Preparation of test solution Take about 1g of fine powder of this product, accurately weigh it, place it in a conical flask, add 50ml of methanol, sonicate for 20 minutes (power 250W, frequency 20kHz), filter. The residue was extracted three times with methanol and the filtrate was combined. The solvent was recovered under reduced pressure to dryness, and the residue was dissolved in a mobile phase and transferred to a 50 ml volumetric flask, diluted with a mobile phase to a mark, shaken, filtered, and the filtrate was taken.
The measurement method accurately draws 10 μl of each of the reference solution and the test solution, and injects into a liquid chromatograph, and the measurement is obtained.
This product is calculated on the basis of dry product, and the mustard base is not less than 0.50% based on sinapine thiocyanate (C 16 H 24 NO 5 ·SCN).
[Processing] Mustards remove impurities. Broken when used.
ã€Properties】 ã€Identification】 ã€Check】 ã€Content determination】The same medicine .
Mustard mustard fried take the net, according to Fried method (Appendix â…¡ D) as a pale yellow to deep yellow fry (fried Brassica alba) or yellow to tan (fried yellow mustard), with a spicy gas. Broken when used.
The surface of this product is light yellow to dark yellow ( fried white mustard) or dark yellow to brown ( fried yellow mustard) , some have focal spots, and some seed coats foam, rupture or fall off.
[Check] herbs with water, not more than 8.0% (Appendix â…¨ H first method).
[Content determination] The same medicine should not be less than 0.40% .
[Identification] [Check] (Total ash, acid-insoluble ash) [Immersion] The same medicine .
Syltech500 High Performance Liquid Chromatograph (single pump configuration/gradient recommended)
1 pump P501 constant current high pressure infusion pump
1.1 Principle of liquid transport: double plunger series reciprocating mode, automatic pulse suppression system, and solvent compression factor program, can automatically compensate flow, liquid delivery is more accurate
1.2 Maximum conveying pressure: 6000PSI or more (about 42MPa or more)
1.3 Flow rate accuracy: 0.1%
1.4 Flow rate range: (0.001-10.000) mL / min minimum increment 0.001mL / min
1.5 Plunger rod cleaning: automatic plunger rod cleaning without additional equipment to protect the plunger rod
1.6 Security: equipped with power-on self-test, high and low voltage alarm and protection
1.7 Gradient System: Binary Gradient Mixing System / Single Pump System
1.7.1 Mixing range: 0 to 100%
1.7.2 Mixing principle: high pressure mixing
1.7.3 Mixed liquid number: greater than or equal to 2 yuan
1.7.4 Degassing device: both internal and external degassing
2 UV detector UV501 UV variable wavelength detector
2.1 Light source: Xenon lamp (optional tungsten lamp) The lamp life is 2000 hours, and the service life is more than 1000 hours.
2.2 Wavelength range: 190 to 720 nm (step increments of 1 nm)
2.3 Wavelength accuracy: <±1nm
2.4 Wavelength reproducibility: <±0.5nm
2.5 Bandwidth: less than 5nm
2.6 Noise: <±2.5*10-5AU (under certain conditions)
2.7 Drift: <±2.5*10-4AU (under certain conditions)
2.8 Flow cell volume: 10ul volume, optical path 10mm
2.9 Absorption range: 0.01AU/V-10AU/V (10 steps total) injection signal control (event), automatic zero adjustment
2.10 Function: With fixed-point wavelength measurement, data processing hardware embedded detector, digital signal direct acquisition and processing function
3 Column: VertexTMXB-C18 4.6*250mm*5um LC column with guard column
4 column oven: 10 degrees to 100 degrees (0.1 degree increments) at room temperature
5 N2010 Pharmacopoeia chromatography workstation: chromatography workstation (to meet the 2010 edition of the pharmacopoeia requirements, the United States made) Chinese and English operating software, support WIN9X/XP/2000/2003 and other operating systems, hardware embedded detector, digital signal direct acquisition and processing
6 Vertex7825i manual injection valve: Vertex7825i manual injection valve (with remote trigger switch), comes with 20UL quantitative, pressure 8000psi, injection times more than 10,000 times