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Conclusion from the results of the study sample of the drug "Ligandrol"

Head of the Laboratory of Chemical Analytical Control and Biotesting of the Federal State Unitary Enterprise Scientific Research Institute of Hygiene, Professional Pathologies and Human Ecology of the Federal Medical-Biological Agency, Doctor of Chemical Sciences

E.I. Savelyev


Samples provided by : Envenom Pharm.
 The purpose of the research: the identification and determination of the active principle in the sample prepara-
 ryta "Ligandrol".
  Object of study: dosage form - capsules.
  Component to be detected: 4 - ((R) -2 - ((R) -2,2,2-trifluoro-1-hydroxyethyl) porrolidin-1-yl) -2-
 trifluoromethyl) benzonitrile.
  Date of receipt of the sample for research: 04/06/2016
  Research Method: High performance liquid chromatography with mass selective detection -
 in high resolution mode.
  Measurement Tools: Acella Liquid Chromatograph with Mass Spectrometry Detector - LTQ
 Orbitrap Velos with electrospray ionization at atmospheric pressure and software
 Xcalibur data management and processing software.
  Measurement Method: Identification of 4 - ((R) -2 - ((R) -2,2,2-trifluoro-1-hydroxyethyl) porrolidin-1-yl) -2-
 trifluoromethyl) benzonitrile in the sample was performed by high performance liquid chromatography method  Fies with mass selective detection in high resolution mode. Component Separation
 samples were carried out on a chromatographic column of a liquid chromatograph with direct detection-  by the separation of separated components by a mass spectrometry detector.
  Brief description of the sample submitted for analysis.
  Trade name of the drug: Ligandrol. Synonyms: Ligandrol, LGDRx, LGD-4033. Dosage Form -
 capsules containing 10 mg of the active ingredient. The active ingredient is a substance with chemical-  By the name of 4 - ((R) -2 - ((R) -2,2,2-trifluoro-1-hydroxyethyl) porrolidin-1-yl) -2-
 trifluoromethyl) benzonitrile.
 Gross formula: С14Н12F6N2O
 Molecular Weight: 338.0854 g/mol
 Appearance of the preparation: powder in a two-color, green-white capsule.
  The active ingredient’s structural formula:


  Sample preparation for analysis.
 A sample of a 10 mg sample was dissolved in 1 ml of water. For a VYGH-MS analysis, the prepared solution
 diluted 100 times.
  Chromatographic Separation Conditions.
 Chromatography column - Zorbax SB-C8, 150 mm long, 4.6 mm in diameter, particle size
 1.8 micron sorbent.
  Mobile Phase:
 - component A - 0.1% solution of formic acid in deionized water;
 - component B - acetonitrile of the category “for gradient VYHH”;
  Mobile Phase Ratio


 The eluent flow rate is 0.4 ml/min;
 Column thermostat temperature: 35 ° С;
 The volume of sample injected for analysis of 5 µl.
  Operating conditions for a mass spectrometric detector.
 Mass spectrometry detector - LTQ Orbitrap Velos with electrospray ionization at
 atmospheric pressure and Xcalibur data management and processing software.
 - Gas flow desiccant 45 cu
 - Auxiliary Gas Flow $ 15
 –The temperature of the gas-drying 300 ° C;
 –Auxiliary flow temperature 380 ° С;
 - The voltage on the capillary 3500V;
 –Detecting in Full Ion Flow Scan Mode (SCAN): Ion Registration in
 m/z range from 50 to 1000 throughout the analysis (with positive ionization).
 The main component was detected by m/z 339.0927, which corresponds positively
 + charged protonated molecular ion [M + H] 4 - ((R) -2 - ((R) -2,2,2-trifluoro-1-hydroxy-e-
 Tyl) porrolidin-1-yl) -2-trifluoromethyl) benzonitrile.


  Figure 1 - HPLC-MS - chromatogram of the sample solution of the drug "Ligandrol"
  and the mass spectrum of the main component.

 Chromatographic peak with a retention time of 5.59 minutes corresponds to the current + [M + H] ion
 substances of the drug "Ligandrol" with a mass number of m/z 339.09266. Deviation from the theoretical
 is less than 0.1 ppm. Measurement error of the exact mass and elemental composition of the ion (difference
 measured mass from the calculated) & lt; 5ppm, identification is authentic.
 A chromatographic peak with a retention time of 4.28 minutes corresponds to an impurity component.
 A quantitative assessment of the main substance was performed by the method of internal normalization. Content
 active ingredient in the sample drug "Ligandrol" was 98%.
 As a result of the study it was found that in the presented sample of the drug "Ligan-
 Drol "the main substance is 4 - ((R) -2 - ((R) -2,2,2-trifluoro-1-hydroxyethyl) porrolidin-1-yl) -2-
 trifluoromethyl) benzonitrile. Estimated content of the analyte in the preparation
 make up