Analysecertifikat: GHK-Cu, batch ATGHK-100-2608-01
GHK-Cu, batch ATGHK-100-2608-01, testet af det uafhængige laboratorium Analyton Labs, certifikat AN-2026-00015 udstedt den 28. august 2026: renhed 99.58 ± 0.15 % ved RP-HPLC, 97.99 mg peptid pr. hætteglas, trifluoracetat < 20 ppm, bakterielle endotoksiner < 0.05 EU/mg, i alt 21 bestemmelser.
- Produkt
- GHK-Cu
- Batch
- ATGHK-100-2608-01
- Certifikatnummer
- AN-2026-00015
- Laboratorium
- Analyton Labs
- Udstedt
- Prøve
- GHK-Cu (copper tripeptide-1), powder, vial labelled 100 mg
Oversigt over resultater, 21 bestemmelser
Metoder og resultater er angivet på engelsk, præcis som laboratoriet har registreret dem.
| Bestemmelse | Metode | Resultat | Specifikation |
|---|---|---|---|
| Appearance | Visual | Blue to blue-violet powder, homogeneous, free of white particles (white particles would be copper-free GHK) | Blue to blue-violet powder |
| Identity | LC-HRMS (ESI+), two conditions, USP <621> principles | In 10 mM ammonium acetate pH 6.5 the complex is seen: m/z 402.1073 [GHK-2H+Cu+H]+, deviation 0.5 ppm, with the 63Cu/65Cu isotope pair 402.107/404.105 at 69:31; in 0.1 % formic acid the complex dissociates and the free ligand is seen: [M+H]+ 341.1932, deviation 0.0 ppm; MS/MS y2 (His-Lys) 284.172, b2 (Gly-His) 195.088; ESI- [M-H]- 339.179 | Theoretical monoisotopic 401.0999 Da from C14H22CuN6O4 ([M+H]+ 402.1071) and 340.1859 Da for GHK from C14H24N6O4 ([M+H]+ 341.1932); difference 60.914 Da = Cu - 2H; deviation <= 10 ppm |
| Purity | RP-HPLC, C18, 214 nm, area %, 0.05 % TFA (the complex dissociates; the GHK ligand is measured) | 99.58 ± 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 0.18 % at RRT 1.08 (± 0.02 %); total impurities 0.42 %, i.e. 0.42 mg per vial; free uncomplexed GHK 1.8 % of area at pH 6.5 (ammonium acetate, 214 nm) | Single <= 0.5 %, total <= 1.0 %; free GHK <= 5 % |
| Impurity profile | RP-HPLC with LC-HRMS assignment | RRT 0.91, 0.12 %, -57.02 Da (des-Gly, His-Lys); RRT 1.08, 0.18 %, +57.02 Da (Gly-Gly-His-Lys, double Gly coupling); RRT 1.19, 0.12 %, +16 Da (His oxidation, 2-oxo-His) | Peaks above 0.05 % reported (ICH Q3B) |
| Complex content | Amino acid analysis after hydrolysis (GHK) and ICP-OES at 324.75 nm (Cu) | 93.50 ± 1.4 % w/w GHK-Cu complex, from GHK 79.20 % w/w and Cu 14.80 ± 0.30 % w/w; molar ratio Cu : GHK = 1.00 (Cu is 15.81 % of the complex mass) | >= 90 % w/w; ratio 0.95 to 1.05 |
| Fill weight | Gravimetric, two vials | 104.8 ± 0.05 mg (second vial 104.0 mg, difference 0.8 %) | Labelled 100 mg |
| Peptide per vial | Calculated from fill weight and net peptide content | 97.99 mg per vial labelled 100 mg, i.e. 98.0 % of label | 95 to 105 % of label |
| Complex composition per vial | Calculated from fill weight, complex content and purity | 98.0 mg of GHK-Cu complex per vial (fill weight × complex content), of which main component 97.6 mg (× purity), GHK 82.5 mg and Cu 15.5 mg | Report only |
| Counter-ion content | Ion chromatography (anion), suppressed conductivity; ICP-OES after SPE for free copper | Acetate 2.00 % w/w (± 0.15 %), 0.14 mol per mol of complex; trifluoroacetate < 20 ppm (LOQ 20 ppm); chloride, sulfate, phosphate < 20 ppm; free uncomplexed Cu2+ 0.10 % w/w | Acetate <= 5.0 %; trifluoroacetate <= 1000 ppm; free Cu2+ <= 0.5 % |
| Water content | Coulometric Karl Fischer, USP <921>, weighed in a dry atmosphere | 4.00 ± 0.20 % w/w (k = 2), i.e. 4.2 mg per vial; hygroscopic powder | <= 8.0 % |
| Mass balance | Complex + counter-ion + water | 93.50 + 2.00 + 4.00 = 99.50 % (± 1.5 %); remainder free Cu2+ 0.10 % and UV-silent residue | Close to 100 % |
| pH | Potentiometric, 10 mg/ml in water, unadjusted | 6.8 (below pH 5 the complex dissociates and the colour fades) | 6.0 to 7.5 |
| Solubility and complex colour | Visual, 50 mg/ml and 1 mg/ml; UV-Vis | >= 50 mg/ml in water and in bacteriostatic water; clear blue-violet solution, free of particles within 30 s; λmax 525 nm (Cu(II) d-d band), A525 = 0.21 at 1 mg/ml in 1 cm, consistent with a 1 : 1 complex | Clear coloured solution |
| Bacterial endotoxins | Kinetic chromogenic LAL, USP <85>, 1 in 100 dilution (Cu2+ inhibits the lysate; dilution validated) | < 0.05 EU/mg (< 5.0 EU per vial; LOQ 0.005 EU/mg) | <= 0.2 EU/mg |
| Sterility | Membrane filtration with rinsing (Cu2+ is antimicrobial; method suitability verified with inoculum), 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>, Cu2+ neutralised with thioglycollate; 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> | Ethanol 120 ppm (crystallisation of the complex); acetonitrile 25 ppm; N,N-dimethylformamide, methanol, dichloromethane, diethyl ether and piperidine each < 10 ppm (LOQ 10 ppm) | ICH Q3C: ethanol <= 5000, acetonitrile <= 410, DMF <= 880, methanol <= 3000, dichloromethane <= 600 ppm |
| Elemental impurities | ICP-MS after microwave digestion (HNO3/H2O2), USP <233>; copper is the active component and is not assessed as an impurity | Cd, Pb, As, Hg < 0.05 µg/g; Co, V < 0.10 µg/g; Ni 0.80 µg/g (companion element of copper salts); Zn 2.1 and Fe 3.5 µg/g for information | ICH Q3D(R2) Class 1 and 2A, parenteral PDE per 100 mg daily: Cd 20, Pb 50, As 150, Hg 30, Co 50, V 100, Ni 200 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-His 0.18 %, D-Lys 0.06 %; Gly achiral; sum of D-forms 0.24 %. His racemises most readily during coupling, which is why D-His sits near the limit and is reported as a number | 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, AHK-Cu, palmitoyl-GHK, free GHK, KPV, Epithalon, protected intermediates (Boc, Trt on His, tBu, Fmoc) and free amino acids (Gly, His, Lys): none above 0.05 % of area | Nothing above 0.05 % |
Filens SHA-256: 091a576f8fafa22fc73da6b105f7754c48252fcc4fc8bbf9b0d8af9541d1e07a
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