AX-2024-005091

Glucagon · 5 mg declared · Shanghai Sigma-Audley New Material Technology Co., Ltd. · lot SSA-2408-F7321

PASSVERIFIED

Report ID: AX-2024-005091
Compound: Glucagon
Compound class: Incretin analogues and co-agonists
Supplier: SSA — Shanghai Sigma-Audley New Material Technology Co., Ltd.
Batch / lot: SSA-2408-F7321
Declared label claim: 5mg
Laboratory: Janoshik Analytical
Assay date: 03 Sep 2024
Submitted: 18 Sep 2024
Quarter: 2024-Q3
Submitter: b.nakamura
Sample provenance: Buyer-sourced

Section 1

Results

Measured against the index acceptance specification for the incretin analogues and co-agonists class. A specification is a decision the index made; a result is a measurement. See where each threshold came from.

Parameter	Method	Result	Unit	Index spec
Purity	RP-HPLC, 30 min gradient, 214 nm	98.53	% area	≥ 98.0	PASS
Total impurities	RP-HPLC, sum of reported peaks	1.47	% area	≤ 2.0	PASS
Largest single impurity	RP-HPLC — glucagon fibril-derived aggregate	0.76	% area	≤ 1.00	PASS
Identity — theoretical monoisotopic mass	calculated from molecular formula	3480.6194	Da	—	NOT TESTED
Identity — observed monoisotopic mass	LC-MS, high resolution (ESI-TOF/QTOF)	3480.6204	Da	—	NOT TESTED
Mass accuracy	observed vs theoretical	+0.3	ppm	± 15	PASS
Total peptide content	by difference from the gravimetric mass balance	86.89	%w/w	—	NOT TESTED
Target-compound content	total peptide content × purity	85.61	%w/w	—	NOT TESTED
Gross fill (as weighed)	five-place balance, under nitrogen	5.76	mg	5 mg declared	NOT TESTED
Recovered target peptide	gross fill × target content	4.931	mg	5 mg claim	NOT TESTED
Recovery against label claim	recovered ÷ claim	98.6	%	90.0 – 110.0	PASS
Water content	Karl Fischer, coulometric, duplicate	7.60	%	≤ 8.0	PASS
Counter-ion (acetate)	anion-exchange ion chromatography	5.23	%	≤ 12.0	PASS
Residual solvent + inorganic residue	estimated — see /methods/residual-solvents-q3c/	0.28	%	—	NOT TESTED
Endotoxin	not ordered on this submission	not determined	—	≤ 5.0	NOT TESTED
Sterility	membrane filtration, USP <71>, 14 d	No growth at 14 d	—	no growth	PASS
Appearance	visual, diffuse light, black and white background	White lyophilised cake, intact	—	white to off-white intact cake	PASS
Reconstitution clarity	reconstituted per submitter procedure	Clear, colourless, no visible particulates	—	clear, no visible particulates	PASS
pH (reconstituted, 1 mg/mL)	potentiometric, two-point calibration	4.73	—	2.5 – 8.0	PASS
Retention time (observed)	RP-HPLC, 30 min gradient	13.75	min	13.61 ± 0.35 (normalised)	PASS
Peak asymmetry (10 % height)	Ph. Eur. 2.2.46	1.01	—	0.80 – 1.50	PASS
Plate count, main peak	N = 5.54 (t/w½)²	65,675	—	≥ 20,000	PASS
Resolution to nearest impurity	vs deamidated Asn28 (+1 Da)	1.64	—	no index criterion	REPORTED

Section 2

Chromatogram and peak integration

The figure is drawn from the table. It is not an independent illustration — if a number in the table changed, the trace would change with it.

Figure 1. RP-HPLC trace, 30 min gradient, 214 nm. Drawn from the peak-integration table below: peak positions are the reported retention times, peak areas are the reported area percentages, peak widths follow the reported plate count of 65,675, and skew follows the reported asymmetry factor of 1.01. Baseline noise is seeded from the report ID and is illustrative. The lower panel is the same trace at a stated vertical expansion with the slow gradient drift subtracted, because at full scale a 0.76 % impurity against a 98.53 % main peak is a line two pixels tall; the main peak runs off-scale there by design.

#	Peak	RT	Area (µV·s)	% area	Δ mass (Da)
1	Glucagon — main peak	13.75	4,788,863	98.53	—
2	glucagon fibril-derived aggregate	16.36	36,938	0.76	0.000
3	deamidated Asn28 (+1 Da)	13.39	20,413	0.42	+0.984
4	Met27 sulfoxide (+16 Da)	12.96	9,235	0.19	+15.995
5	des-His1 (−137 Da)	12.81	4,860	0.10	-137.059
Closure check — purity + Σ impurities				100.00	CLOSES

Reporting threshold 0.05 % area. Peaks below it are not reported and are therefore excluded from the total, which overstates purity by their sum — see peak integration.

Section 3

Mass spectrum and identity

Theoretical monoisotopic mass 3480.6194 Da, computed from C153H225N43O49S. All ppm figures on this site are against monoisotopic values — see why that matters.

Figure 2. ESI charge-state envelope, high-resolution instrument. Sticks are placed at m/z = (M + z × 1.007276)/z for the observed neutral mass of 3480.6204 Da. Sodium (+21.982/z) and potassium (+37.956/z) adducts are shown where the parent charge state exceeds 25 % relative abundance; they are adducts of the same molecule and are not impurities.

Charge	Theoretical m/z	Observed m/z	Δ m/z	Rel. abundance (%)
5+	697.1312	697.1314	0.0002	8.2
4+	871.1621	871.1624	0.0003	54.7
3+	1161.2137	1161.2141	0.0004	100.0
2+	1741.3170	1741.3175	0.0005	51.8

Section 4

Gravimetric mass balance

Water, counter-ion, residual and total peptide content are exhaustive and mutually exclusive categories. They must account for 100 % of the cake mass. The index closes this to within 0.02 pp and the build asserts it.

Component	Determination	%w/w of cake
Water	Karl Fischer	7.60
Counter-ion (acetate)	ion chromatography	5.23
Residual solvent + inorganic residue	estimated	0.28
Total peptide content	by difference	86.89
Total		100.00 CLOSES

Supplier certificate, as declared

The supplier's own figures for this lot, beside the independent measurement. Divergence is assessed against the batch median, not against this single report — see rule AX-R05.

Figure	Supplier COA	This report	Index note
Purity (% area)	98.22	98.53	divergence -0.31 pp vs batch median
Total impurities (% area)	1.78	1.47
Largest single impurity (% area)	0.96	0.76
Water (%)	not stated	7.60
Counter-ion (%)	3.8	5.23
Peptide content (%w/w)	92.1	86.89
Endotoxin (EU/mg)	0.25	not determined
Method stated on certificate	YES	—	column, gradient and wavelength given

Section 5

Provenance and caveats

Where a sample came from changes the weight of the evidence. The index treats it as a first-class field.

Sample provenance: Buyer-sourced
Evidentiary weight: Strongest available evidence in this index.
Chain of custody: Retail purchase → submitter (−20 °C, 32 d) → laboratory (courier, dry ice, 5 d) → assay.
Assay date: 03 Sep 2024
Submitted to the index: 18 Sep 2024
Laboratory: Janoshik Analytical, Ostrava, Czechia
Method basis: 30 min gradient · high-resolution MS
Verification status: VERIFIED

What this report does not establish

That the material is free of bacterial endotoxin. Endotoxin was not measured. No chromatographic result bears on it.
That any other vial in the same lot has the same composition. One vial was tested. Within-lot vial-to-vial variation in this index has a median of 0.28 pp and a 90th percentile of 0.74 pp.
That any other lot from the same supplier has the same composition. Batch-to-batch variation is larger than within-batch variation for every supplier here.
That the material is suitable for administration to a human or an animal. These are research compounds. No result on this site is a safety assessment and the index takes no position on use.
That the material was manufactured by the supplier that sold it. Contract synthesis is normal in this market and twenty-nine batches in the index fingerprint to a bulk from a different company than the one named on the label.

Section 6

Annotations 1

Signed technical comments from index contributors. Not a discussion forum — annotations question or contextualise the result, and the data team replies where a reply is warranted.

charge_envelope18 Sep 2024

Base peak lands where the charge-state arithmetic says it should for a species of this mass. That agreement is a check on the deconvolution rather than on the material, and it passes.

Section 7

Related records

Same batch — lot SSA-2408-F7321 n=1

This is the only report on this lot. One report is not a batch characterisation.

Batch rollup and reproducibility assessment →

Cross-sections

Other recent Glucagon records in the index.
Report	Supplier	Lot	Lab	Quarter	Purity %	Water %	Recovery %	Provenance	Result
AX-2026-042421	Homopeptide	HOMO-2602-V3961	PeptideMeter	2026-Q2	99.38	6.63	95.7	Buyer-sourced	PASS
AX-2026-042411	Homopeptide	HOMO-2602-V3961	Janoshik	2026-Q2	99.00	6.22	98.9	Buyer-sourced	PASS
AX-2026-042413	Homopeptide	HOMO-2602-V3961	Janoshik	2026-Q2	99.25	6.65	—	Buyer-sourced	PASS
AX-2026-042416	Homopeptide	HOMO-2602-V3961	Janoshik	2026-Q2	99.60	6.15	—	Buyer-sourced	PASS
AX-2026-042419	Homopeptide	HOMO-2602-V3961	Janoshik	2026-Q2	99.21	6.84	—	Buyer-sourced	PASS
AX-2026-042418	Homopeptide	HOMO-2602-V3961	Medutest	2026-Q2	99.20	6.31	97.8	Buyer-sourced	PASS
AX-2026-042412	Homopeptide	HOMO-2602-V3961	Janoshik	2026-Q2	99.32	6.35	102.2	Buyer-sourced	PASS
AX-2026-042422	Homopeptide	HOMO-2602-V3961	Janoshik	2026-Q2	99.23	6.89	—	Buyer-sourced	PASS

Other recent SSA records in the index.
Report	Compound	Lot	Lab	Quarter	Purity %	Water %	Recovery %	Provenance	Flags	Result
AX-2026-043135	BPC-157	SSA-2601-N6863	Nordanalyt	2026-Q2	98.16	4.66	92.8	Buyer-sourced	1	MARGINAL
AX-2026-043160	GHK-Cu	SSA-2604-V7731	Janoshik	2026-Q2	98.01	4.02	91.8	Buyer-sourced	0	PASS
AX-2026-043157	GHK-Cu	SSA-2604-V7731	Medutest	2026-Q2	99.19	5.14	—	Supplier-supplied	0	PASS
AX-2026-043141	BPC-157	SSA-2601-N6863	Janoshik	2026-Q2	98.06	4.06	94.6	Buyer-sourced	1	MARGINAL
AX-2026-043154	GHK-Cu	SSA-2604-V7731	PeptideMeter	2026-Q2	97.82	4.82	101.6	Buyer-sourced	0	PASS
AX-2026-043137	BPC-157	SSA-2601-N6863	PeptideMeter	2026-Q2	98.17	4.14	—	Buyer-sourced	1	MARGINAL
AX-2026-043162	GHK-Cu	SSA-2604-V7731	Janoshik	2026-Q2	98.50	4.36	—	Supplier-supplied	0	PASS
AX-2026-043134	BPC-157	SSA-2601-N6863	Medutest	2026-Q2	97.89	4.01	—	Buyer-sourced	1	FAIL