VendorInvestigate result on a Nantong dulaglutide lot lands 0.9 points above the supplier’s stated figure

A peptide content determination commissioned by the Journal on a 20 mg dulaglutide vial from QYB has returned 98% of the labelled mass, the balance being the counter-ion and residual water that every lyophilised salt carries. Chromatographic purity on the same vial was above 96.5%. The two numbers measure different things, and this is one of the few certificates in the trade to print both.

Content by elemental nitrogen determination returned 98% of the labelled nominal mass, which on a 20 mg vial corresponds to roughly 6.86 mg of peptide rather than the labelled figure. The remainder is accounted for by counter-ion, residual water and residual solvent, none of which is visible chromatographically.

The Journal purchased 8 vials from the same lot at retail and had four of them analysed separately, in order to distinguish vial-to-vial variation from method variation. Vial-to-vial agreement was within 0.4 percentage points. Method-to-method disagreement was an order of magnitude larger.

Discrepancies of one to two percentage points between a supplier’s figure and an independent determination are common and usually explicable: a faster gradient resolves fewer impurities, a higher integration threshold discards more small peaks, and a wider solvent-front exclusion window removes early-eluting fragments from the calculation altogether. None of that is misconduct. All of it is invisible unless the method is disclosed.

"Content is the number that matters if you are doing arithmetic with a vial, and content is the number nobody sells," said Dr Wenjun Xie, process chemist and peptide manufacturing consultant. "Purity is what you can afford. Content is what you need."

QYB’s dossier has been updated with this determination and with the company’s response to it. The dossier’s ordering box records the lead times, the minimum quantities and what a buyer should ask for at the point of order.