Πιστοποιητικό ανάλυσης: Pinealon (Glu-Asp-Arg), παρτίδα ATPIN-20-2609-01
Pinealon (Glu-Asp-Arg), παρτίδα ATPIN-20-2609-01, αναλύθηκε από το ανεξάρτητο εργαστήριο Analyton Labs, πιστοποιητικό AN-2026-00016 που εκδόθηκε στις 15 Οκτωβρίου 2026: καθαρότητα 99.62 ± 0.15 % με RP-HPLC, 19.80 mg πεπτιδίου ανά φιαλίδιο, τριφθοροξικό οξύ (TFA) < 20 ppm, βακτηριακές ενδοτοξίνες < 0.05 EU/mg, συνολικά 20 προσδιορισμοί.
- Προϊόν
- Pinealon (Glu-Asp-Arg)
- Παρτίδα
- ATPIN-20-2609-01
- Αριθμός πιστοποιητικού
- AN-2026-00016
- Εργαστήριο
- Analyton Labs
- Ημερομηνία έκδοσης
- Δείγμα
- Pinealon (Glu-Asp-Arg), lyophilised powder, vial labelled 20 mg
Σύνοψη αποτελεσμάτων, 20 προσδιορισμοί
Οι μέθοδοι και τα αποτελέσματα δίνονται στα αγγλικά, ακριβώς όπως τα κατέγραψε το εργαστήριο.
| Προσδιορισμός | Μέθοδος | Αποτέλεσμα | Προδιαγραφή |
|---|---|---|---|
| Appearance | Visual | White to off-white lyophilised powder, free of visible particles | White to off-white powder |
| Identity | LC-HRMS, ESI+ and ESI-, USP <621> principles | [M+H]+ 419.1886, deviation 0.2 ppm; [M+2H]2+ 210.098; [M-H]- 417.1744, deviation 1.2 ppm; MS/MS y1 (Arg) 175.119, b2 (Glu-Asp) 245.077, y2 (Asp-Arg) 290.146: residue order Glu-Asp-Arg confirmed | Theoretical monoisotopic 418.1812 Da from C15H26N6O8; [M+H]+ 419.1885, [M-H]- 417.1739; deviation <= 10 ppm |
| Purity | RP-HPLC, C18 polar-endcapped, 214 nm, area %, 0.1 % TFA | 99.62 ± 0.15 % (k = 2) | >= 99.0 % |
| Related substances | RP-HPLC, 214 nm; LOD 0.01 %, LOQ 0.03 %, reporting threshold 0.05 % | Largest single impurity 0.11 % at RRT 0.94 (± 0.02 %); total impurities 0.38 %, i.e. 0.076 mg per vial | Single <= 0.5 %, total <= 1.0 % |
| Impurity profile | RP-HPLC with LC-HRMS assignment | RRT 0.86, 0.10 %, -129.04 Da (des-Glu, Asp-Arg); RRT 0.94, 0.11 %, same mass (beta-Asp2 isomer, isoAsp); RRT 1.07, 0.09 %, -18.01 Da (pyroGlu1-Asp-Arg, N-terminal cyclisation); RRT 1.15, 0.08 %, +129.04 Da (Glu-Glu-Asp-Arg, double Glu coupling) | Peaks above 0.05 % reported (ICH Q3B) |
| Net peptide content | Amino acid analysis after acid hydrolysis (AAA) | 81.50 ± 1.2 % w/w (k = 2); a tripeptide with Arg binds more counter-ion and water per unit mass than a long peptide, hence the lower limit | >= 75 % |
| Fill weight | Gravimetric, two vials | 24.3 ± 0.05 mg (second vial 24.6 mg, difference 1.2 %) | Labelled 20 mg |
| Peptide per vial | Calculated from fill weight and net peptide content | 19.80 mg per vial labelled 20 mg, i.e. 99.0 % of label | 95 to 105 % of label |
| Counter-ion content | Ion chromatography (anion), suppressed conductivity | Acetate 12.30 % w/w (± 0.6 %), i.e. 3.0 mg per vial, 1.05 mol per mol at two basic sites (Glu1 N-terminus and Arg3 guanidine); trifluoroacetate < 20 ppm (LOQ 20 ppm); chloride and phosphate < 20 ppm | Acetate <= 15 %; trifluoroacetate <= 1000 ppm |
| Water content | Coulometric Karl Fischer, USP <921> | 5.60 ± 0.28 % w/w (k = 2), i.e. 1.4 mg per vial | <= 8.0 % |
| Mass balance | Peptide + counter-ion + water | 81.50 + 12.30 + 5.60 = 99.40 % (± 1.4 %) | Close to 100 % |
| pH | Potentiometric, 20 mg/ml in water | 4.9 (acidic peptide as acetate) | 4.0 to 5.5 |
| Solubility | Visual, 20 mg/ml and 1 mg/ml | >= 20 mg/ml in water and in bacteriostatic water; clear, colourless, free of particles within 15 s | Clear solution |
| Bacterial endotoxins | Kinetic chromogenic LAL, USP <85> | < 0.05 EU/mg (< 1.0 EU per vial; LOQ 0.005 EU/mg) | <= 0.5 EU/mg |
| Sterility | Membrane filtration, USP <71>; fluid thioglycollate 30 to 35 °C and soya bean casein digest 20 to 25 °C | No growth after 14 days, 2 vials | No growth |
| Microbial enumeration | Plate count, USP <61>; specified organisms, USP <62> | TAMC < 10 CFU/g, TYMC < 10 CFU/g; Escherichia coli, Salmonella, Staphylococcus aureus and Pseudomonas aeruginosa absent in 1 g | TAMC <= 1000 CFU/g, TYMC <= 100 CFU/g; specified organisms absent |
| Residual solvents | Headspace GC, USP <467> | Acetonitrile 22 ppm; N,N-dimethylformamide, methanol, dichloromethane, diethyl ether, diisopropyl ether and piperidine each < 10 ppm (LOQ 10 ppm) | ICH Q3C: acetonitrile <= 410, DMF <= 880, methanol <= 3000, dichloromethane <= 600, ethers <= 5000 ppm |
| Elemental impurities | ICP-MS after microwave digestion (HNO3/H2O2), USP <233> | Cd, Pb, As, Hg < 0.05 µg/g; Co, V, Ni < 0.10 µg/g, all below LOQ | ICH Q3D(R2) Class 1 and 2A, parenteral PDE per 20 mg daily: Cd 100, Pb 250, As 750, Hg 150, Co 250, V 500, Ni 1000 µg/g |
| Chiral purity (D-amino acids) | Acid hydrolysis (6 M DCl in D2O, 110 °C, 24 h), Marfey's derivatisation (FDAA), LC-MS | D-Asp 0.10 %, D-Glu 0.09 %, D-Arg 0.04 %; sum of D-forms 0.23 %. All three residues are chiral; an enantiomer has the same mass and the same achiral retention time, so this determination is decisive for a tripeptide | Each D-amino acid <= 0.2 %, sum of D-forms <= 0.5 % |
| Compound screening | LC-HRMS full scan m/z 100 to 2000, both polarities, against reference standards | Fentanyl and analogues, Epithalon (AEDG), Vilon (KE), Thymogen (EW), Semax, Selank, protected intermediates (tBu on Glu/Asp, Pbf on Arg, Fmoc, Boc) and free amino acids (Glu, Asp, Arg): none above 0.05 % of area | Nothing above 0.05 % |
SHA-256 του αρχείου: 7583f2b6609f98ab631f40f983f93865520111159ae0c030cb4edd5be752535d
Ερευνητικό υλικό. Το πιστοποιητικό περιγράφει τις ιδιότητες της παρτίδας και όχι την καταλληλότητά της για οποιαδήποτε χρήση σε ανθρώπους ή ζώα.
