Analīzes sertifikāts: Tirzepatide, partija ATTZP-05-2607-01
Tirzepatide, partija ATTZP-05-2607-01, pārbaudījusi neatkarīgā laboratorija Analyton Labs, sertifikāts AN-2026-00014 izsniegts 2026. gada 1. augusts: tīrība 99.25 ± 0.20 % (RP-HPLC), 4.92 mg peptīda uz flakonu, trifluoracetāts < 20 ppm, bakteriālie endotoksīni < 0.05 EU/mg, kopā 20 noteikšanas.
- Produkts
- Tirzepatide
- Partija
- ATTZP-05-2607-01
- Sertifikāta numurs
- AN-2026-00014
- Laboratorija
- Analyton Labs
- Izsniegšanas datums
- Paraugs
- Tirzepatide, lyophilised powder, vial labelled 5 mg
Rezultātu kopsavilkums, 20 noteikšanas
Metodes un rezultāti ir norādīti angļu valodā tieši tā, kā tos reģistrējusi laboratorija.
| Noteikšana | Metode | Rezultāts | Specifikācija |
|---|---|---|---|
| Appearance | Visual | White to off-white lyophilised cake, free of visible particles | White to off-white powder or cake |
| Identity | LC-HRMS (ESI+), USP <621> principles | Deconvoluted monoisotopic mass 4810.529 Da, deviation 0.8 ppm (0.004 Da); observed m/z 1604.516 (3+), 1203.638 (4+), 963.112 (5+); charge envelope 3+ to 6+ | Theoretical monoisotopic 4810.525 Da from C225H348N48O68 (average 4813.5 Da); expected m/z 1604.516 (3+), 1203.638 (4+), 963.112 (5+); deviation <= 10 ppm |
| Purity | RP-HPLC, C18, 214 nm, area % | 99.25 ± 0.20 % (k = 2) | >= 99.0 % |
| Related substances | RP-HPLC, 214 nm; LOD 0.01 %, LOQ 0.03 %, reporting threshold 0.05 % | Largest single impurity 0.21 % at RRT 1.03 (± 0.02 %); total impurities 0.75 %, i.e. 0.038 mg per vial | Single <= 0.5 %, total <= 1.0 % |
| Impurity profile | RP-HPLC with LC-HRMS assignment | RRT 0.93, 0.12 %, -18 Da (Asp9 or Asp15 succinimide); RRT 0.97, 0.17 %, same mass (isoAsp9 or isoAsp15); RRT 1.03, 0.21 %, +0.98 Da (deamidation of Gln19 or Gln24); RRT 1.06, 0.09 %, -28.03 Da (C18 diacid analogue, acyl chain short by C2H4); RRT 1.12, 0.16 %, +16 Da (Trp25 or Tyr oxidation) | Peaks above 0.05 % reported (ICH Q3B) |
| Net peptide content | Amino acid analysis after acid hydrolysis (AAA), eight stable residues | 94.80 ± 1.3 % w/w (k = 2) | >= 90 % |
| Fill weight | Gravimetric, two vials | 5.19 ± 0.05 mg (second vial 5.15 mg, difference 0.8 %) | Labelled 5 mg |
| Peptide per vial | Calculated from fill weight and net peptide content | 4.92 mg per vial labelled 5 mg, i.e. 98.4 % of label | 95 to 105 % of label |
| Counter-ion content | Ion chromatography (anion), suppressed conductivity | Acetate 2.40 % w/w (± 0.15 %), i.e. 0.12 mg per vial, 1.9 mol per mol at two basic sites (Tyr1 N-terminus and Lys16; Lys20 carries the acyl chain); trifluoroacetate < 20 ppm (LOQ 20 ppm); chloride and phosphate < 20 ppm | Acetate <= 5.0 %; trifluoroacetate <= 1000 ppm |
| Water content | Coulometric Karl Fischer, USP <921> | 2.60 ± 0.15 % w/w (k = 2), i.e. 0.13 mg per vial | <= 5.0 % |
| Mass balance | Peptide + counter-ion + water | 94.80 + 2.40 + 2.60 = 99.80 % (± 1.3 %) | Close to 100 % |
| pH | Potentiometric, 10 mg/ml in water | 6.8 (acidic peptide, pI 4.4, unbuffered) | 6.0 to 7.5 |
| Solubility | Visual, 10 mg/ml and 1 mg/ml | >= 10 mg/ml in water and in bacteriostatic water; clear, colourless, free of particles within 60 s (lipidated peptide wets slowly); no opalescence after 24 h at 2 to 8 °C | Clear solution |
| Bacterial endotoxins | Kinetic chromogenic LAL, USP <85> | < 0.05 EU/mg (< 0.25 EU per vial; LOQ 0.005 EU/mg) | <= 1.0 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 38 ppm; N,N-dimethylformamide, methanol, dichloromethane, diethyl ether, diisopropyl ether, tert-butyl methyl 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 5 mg daily: Cd 400, Pb 1000, As 3000, Hg 600, Co 1000, V 2000, Ni 4000 µg/g |
| Chiral purity (D-amino acids) | Acid hydrolysis (6 M DCl in D2O, 110 °C, 24 h; Trp after alkaline hydrolysis), Marfey's derivatisation (FDAA), LC-MS | D-Tyr 0.05 %, D-Ser 0.05 %, D-Glu (Glu + Gln) 0.04 %, D-Phe 0.04 %, D-Thr 0.03 %, D-Asp 0.03 %, D-Ile 0.02 %, D-Leu 0.02 %, others < 0.02 %; Aib and Gly achiral; sum of D-forms 0.28 % | 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, semaglutide, liraglutide, retatrutide, GLP-1 (7-37), GIP (1-42), cagrilintide, protected intermediates (tBu, Boc, Trt, Pbf, Fmoc, protected acyl chain) and free amino acids: none above 0.05 % of area | Nothing above 0.05 % |
Faila SHA-256: 4d04161d08e034e12efe7293d46d5a7a26d15fd91c4fa4ff65de800beeb7e0bb
Pētniecības materiāls. Sertifikāts apraksta partijas īpašības, nevis tās piemērotību lietošanai cilvēkiem vai dzīvniekiem.
