D-Phenylalanine CAS 673-06-3 (H-D-Phe-OH) Assay 98.0~102.0% Factory 50MT/Month

1. Appearance-- Visual inspection
2. Specific rotation-- Specific rotation is measured in accordance with GB/T613-1988
Sample preparation: Accurately weigh the 0.5000g sample and move it to a clean and dry 50ml volumetric bottle, add 20ml water, cover the bottle, shake it to dissolve, and then dilute it to the scale with water.
Test: Adjust the zero of the gyroscope before the test, then load the test tube with the sample solution, record the rotation Angle, and calculate the specific rotation of the sample with the following formula.
[а]D20 = (r×50) ÷(L×W)
Where:
[а]D20: Specific optical rotation at 20℃ of sample solution
r: Optical rotation observed at 20℃ for the sample solution
50: Volume of prepared sample solution (ml)
w: Sample weight (g)
L: Optical rotation tube length (dm)
3. Burning residue
Take about 1g of this product and heat it at 600℃, heat it until it is completely ashes according to the regulation of Appendix Ⅷ N of Part II of CP2010 Edition, add 0.5-1.0ml concentrated sulfuric acid and heat it (700℃-800℃) to constant weight.
3.1 "Incandescent residue" in this Method (Chinese Pharmacopoeia 2005 Edition, Part II Appendix Ⅷ N) refers to the metal oxides or sulfates left over after the drugs (mostly organic compounds) are heated until completely ash, then sulfuric acid is added 0.5 ~ 1.0ml and incandesced (700 ~ 800℃) to constant weight.
4 Chiral purity (HPLC)
Instruments: High performance liquid chromatography, PDA detector. Electronic analytical balance, reagent; Level of chromatography
Chromatographic conditions: Column: Astec CHIROBIOTICTMT HPLC Column 250X4.6mm,5ul, detection wavelength, flow rate, sample size :10 u L(reference) thinner: water, data collection time :20.00min.
Sample determination: The sample was analyzed according to the following sampling procedure :1 needle of blank solution and 1 needle of DL-phenylalanine reference.
1 needle sample solution,
Results Calculation: HPLC content was determined to be less than 0.5% according to peak area normalization and blank deduction.
5. Dry and weightless
5.1 Instruments:
Thermostatic drying oven, 1/10,000 balance.
5.2 Procedure:
In a flat weighing bottle with a constant weight and over-drying ground mouth cover, weigh 1 gram (accurate to 0.0001 gram) of the sample. The sample should be evenly spread at the bottom of the weighing bottle with a thickness of no more than 10mm, put in a thermostatic electric drying oven, dry at 105-110 ℃ for 3 hours, and then move into the drying room to cool to room temperature for weighing.
Calculation: Dry weight loss %= (M1-M2) ÷M×100
Where: M1: mass of sample and measuring bottle before drying, grams
M2: Mass of sample and measuring bottle after drying, in grams
M: Sample mass, grams
Step 6: Content
6.1 Instruments
High performance liquid chromatography, PDA detector.
Electronic analytical balance
6.2 Reagents
Acetonitrile (chromatographic grade), TFA(chromatographic grade)
6.3 Chromatographic Conditions
6.3.1 Column: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Detection wavelength: INC220nm
Flow rate :1.0mL/min
Sample size: 10μL(for reference)
Thinner: Acetonitrile
Data collection time: 20.00min
6.4 Mobile phase preparation
Mobile phase A (0.1% trifluoroacetic acid water): precision absorption 2. Dilute Oml trifluoroacetic acid with water to 2000m1, mix well, and degas;
Mobile phase B(0.1% acetonitrile trifluoroacetic acid): precise absorption 2.Oml trifluoroacetic acid was diluted to 2000m1 with acetonitrile, mixed and deggated;
6.5 Mobile phase gradient program
Time (min) A% B%
0.00 90 10
12.00 10 90
15.00 10 90
15.01 90 10
20.00 90 10
6.6 Preparation of sample solution
Weigh and dissolve 0.1g sample with acetonitrile, dilute to 100m1, shake well for use, or the same concentration. Prepare two samples in parallel.
6.7 Sample Determination
Analyze the sample according to the following sampling procedure:
More than 1 injection of blank solution
1 needle sample solution 1#
1 needle sample solution 2#
6.8 Result Calculation
2.8.1 The peak area normalization method was used to calculate the HPLC purity by deducting blank space.
2.8.2 The relative mean deviation of the purity of two needles shall not be greater than 1%
2.8.3 If the results of both injections meet the acceptance criteria, the average purity is taken as the final result.