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mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and what a mass shift of one, eighteen or one hundred and twenty-eight daltons tells you about what went wrong.

52 questions · sorted by votes · page 1 of 3

41 votes 5 answers35k views
Would identity confirmation by mass spectrometry distinguish aspartimide formation from a synthesis impurity in a GLP-1 receptor agonist?

The particulars: identity confirmation by mass spectrometry · aspartimide formation · a GLP-1 receptor agonist. The comparison I want does not seem to exist anywhere…

peptide-mapping
peptide-mapping

Enzymatic digestion followed by LC-MS/MS to confirm sequence rather than just mass. The method that catches a scrambled sequence or a D-amino-acid…

103 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
asked by mass_shift_18 9.7k · 19 months ago
39 votes 5 answers65k views
How do I compute the +4 charge state m/z for a peptide of 4207.2 Da?

The specifics, since they change the answer: +4 · 4207.2 Da. I would like the arithmetic checked rather than the conclusion asserted. I have deliberately not used an…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by dermot_kiely 12k · 2.0 years ago
39 votes 5 answers33k views
Would a sterility test distinguish dimerisation from a synthesis impurity in tirzepatide?

The case in front of me: a sterility test · dimerisation · tirzepatide. I have used one of these for a while and I am considering switching, which requires a reason.…

peptide-mapping
peptide-mapping

Enzymatic digestion followed by LC-MS/MS to confirm sequence rather than just mass. The method that catches a scrambled sequence or a D-amino-acid…

103 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
sterility
sterility

Sterility as a test result rather than an adjective. Covers what a sterility test actually measures, why "sterile filtered" on a document is close…

142 questions
tirzepatide
tirzepatide

A dual GIP and GLP-1 receptor agonist. Questions here cover the SURPASS and SURMOUNT programmes, the practical differences from a pure GLP-1…

370 questions
asked by assay_blank 45k · 19 months ago
35 votes 5 answers65k views
What does identity confirmation by mass spectrometry add for ecnoglutide that a purity figure does not?

The specifics, since they change the answer: identity confirmation by mass spectrometry · ecnoglutide. I am trying to choose between two options that are usually…

content-assay
content-assay

Quantified content: how many milligrams of peptide are actually in the vial, measured against a calibrated reference standard. A separate test…

476 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
coa
coa

Certificates of analysis: what fields a useful one carries, how to tell a real analytical report from a marketing document, batch and lot…

771 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
ecnoglutide
ecnoglutide

A long-acting GLP-1 receptor agonist with a cAMP-biased signalling profile. A niche tag, mostly used for mechanism questions about biased agonism…

223 questions
asked by pieter_maas 14k · 2.3 years ago
35 votes5 answers31k views
How do I compute the +2 charge state m/z for a peptide of 4207.2 Da?

What I have: +2 · 4207.2 Da. This should be a straightforward calculation and I keep getting two different answers. The numbers are arbitrary; the method is what I am…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by liam_bracken 6.9k · 22 months ago
34 votes 5 answers43k views
How many vials from a BCH lot should I send for identity confirmation by mass spectrometry?

Details up front: BCH · identity confirmation by mass spectrometry. I have worked this out and I would like someone to find the error, because I suspect there is one.…

batch-testing
batch-testing

Testing at the batch or lot level: sampling plans, how many vials from a lot need testing to say anything about the lot, and the difference…

910 questions
coa
coa

Certificates of analysis: what fields a useful one carries, how to tell a real analytical report from a marketing document, batch and lot…

771 questions
cost-analysis
cost-analysis

Cost arithmetic done honestly: cost per milligram after dead-space loss, list versus net price, comparing a multi-dose vial to a fixed-dose pen,…

260 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
asked by fresh_bac 9.7k · 18 months ago
34 votes 5 answers38k views
How many vials from a QSC lot should I send for identity confirmation by mass spectrometry?

Details up front: QSC · identity confirmation by mass spectrometry. I have worked this out and I would like someone to find the error, because I suspect there is one.…

batch-testing
batch-testing

Testing at the batch or lot level: sampling plans, how many vials from a lot need testing to say anything about the lot, and the difference…

910 questions
coa
coa

Certificates of analysis: what fields a useful one carries, how to tell a real analytical report from a marketing document, batch and lot…

771 questions
cost-analysis
cost-analysis

Cost arithmetic done honestly: cost per milligram after dead-space loss, list versus net price, comparing a multi-dose vial to a fixed-dose pen,…

260 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
asked by seven_day_half 31k · 16 months ago
31 votes 5 answers35k views
How do I compute the +5 charge state m/z for a peptide of 4113.6 Da?

Conditions: +5 · 4113.6 Da. I want the working, not the result — I need to be able to redo it with different numbers. I care about the precision as well as the value…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by w_okoye 43k · 2.0 years ago
28 votes 5 answers38k views
Would peptide mapping distinguish oxidation from a synthesis impurity in cagrilintide?

Concretely: peptide mapping · oxidation · cagrilintide. I am trying to choose between two options that are usually discussed as though only one exists. I am not…

peptide-mapping
peptide-mapping

Enzymatic digestion followed by LC-MS/MS to confirm sequence rather than just mass. The method that catches a scrambled sequence or a D-amino-acid…

103 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
amylin
amylin

Amylin and its analogues, most prominently cagrilintide, as a satiety mechanism orthogonal to incretin signalling. Includes the pharmacology of…

237 questions
asked by kofi_mensah 18k · 14 months ago
28 votes5 answers13k views
How many vials from an ERP lot should I send for identity confirmation by mass spectrometry?

For reference: ERP · identity confirmation by mass spectrometry. I have worked this out and I would like someone to find the error, because I suspect there is one. My…

batch-testing
batch-testing

Testing at the batch or lot level: sampling plans, how many vials from a lot need testing to say anything about the lot, and the difference…

910 questions
coa
coa

Certificates of analysis: what fields a useful one carries, how to tell a real analytical report from a marketing document, batch and lot…

771 questions
cost-analysis
cost-analysis

Cost arithmetic done honestly: cost per milligram after dead-space loss, list versus net price, comparing a multi-dose vial to a fixed-dose pen,…

260 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
asked by plunger_stop 13k · 7 months ago
28 votes 3 answers12k views
If the mass spec matches exactly, why is that not proof the vial is pure?

A vendor sent me a report showing a clean deconvolved mass at 4113.6 for semaglutide with, in their words, "no impurity peaks detected". Their sales copy turns that…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
coa
coa

Certificates of analysis: what fields a useful one carries, how to tell a real analytical report from a marketing document, batch and lot…

771 questions
hplc
hplc

Reverse-phase high-performance liquid chromatography, the workhorse purity method. Column chemistry, mobile-phase choice, gradient slope,…

503 questions
janoshik
janoshik

Janoshik Analytical, an independent third-party testing laboratory widely used by this community for HPLC purity, identity and quantified content…

139 questions
asked by net_peptide 12k · 20 months ago
27 votes 5 answers51k views
How do I compute the +5 charge state m/z for a peptide of 4813.5 Da?

The case in front of me: +5 · 4813.5 Da. I want the working, not the result — I need to be able to redo it with different numbers. I care about the precision as well…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by leah_ferrers 12k · 22 months ago
27 votes 5 answers27k views
How do I compute the +4 charge state m/z for a peptide of 3751.0 Da?

The specifics, since they change the answer: +4 · 3751.0 Da. I would rather understand the derivation than memorise the outcome. Two people I asked gave two answers…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by lyoph_cake 78k · 18 months ago
25 votes1 answer19k views
How do I compute the +4 charge state m/z for a peptide of 4731.3 Da?

For reference: +4 · 4731.3 Da. I would rather understand the derivation than memorise the outcome. Two people I asked gave two answers that differ by a factor of ten,…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by gradient_slope 46k · 13 months ago
24 votes0 answers19k views
Is identity confirmation by mass spectrometry on one vial from a twenty-person split enough for the whole split?

The specifics, since they change the answer: identity confirmation by mass spectrometry · a twenty-person split. I would like to define my thresholds before I have a…

group-buy
group-buy

Pooled purchasing: how the economics work, what trust structure a pool needs, splitting a single tested lot, and the failure modes when the…

41 questions
batch-testing
batch-testing

Testing at the batch or lot level: sampling plans, how many vials from a lot need testing to say anything about the lot, and the difference…

910 questions
coa
coa

Certificates of analysis: what fields a useful one carries, how to tell a real analytical report from a marketing document, batch and lot…

771 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
asked by jonas_ekstrom 12k · 20 months ago
22 votes 5 answers30k views
Would an endotoxin test distinguish racemisation from a synthesis impurity in survodutide?

The case in front of me: an endotoxin test · racemisation · survodutide. I suspect the honest answer is that it depends, in which case I would like to know on what.…

peptide-mapping
peptide-mapping

Enzymatic digestion followed by LC-MS/MS to confirm sequence rather than just mass. The method that catches a scrambled sequence or a D-amino-acid…

103 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
endotoxin
endotoxin

Bacterial endotoxin: LAL and kinetic chromogenic methods, how an endotoxin limit is derived from a dose, why endotoxin survives autoclaving, and…

23 questions
survodutide
survodutide

A GLP-1 and glucagon receptor dual agonist with a substantial published MASH dataset. Use this tag for its hepatic endpoints, its dose ladder, and…

225 questions
asked by retest_please 9.7k · 15 months ago
22 votes 5 answers18k views
When is LC-MS worth its cost over HPLC plus a separate mass check?

The method section is present, which is unusual enough that I want to make use of it. I suspect the honest answer is that it depends, in which case I would like to…

lc-ms
lc-ms

Liquid chromatography coupled to mass spectrometry: separation and identification in one run, and the method of choice when you need to know not…

10 questions
hplc
hplc

Reverse-phase high-performance liquid chromatography, the workhorse purity method. Column chemistry, mobile-phase choice, gradient slope,…

503 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
asked by swab_and_wait 13k · 12 months ago
22 votes3 answers6.5k views
When is LC-MS/MS peptide mapping worth paying for instead of a plain intact mass?

I have been quoted roughly four times the price of a purity-plus-identity panel for something described as "tryptic digest with LC-MS/MS peptide mapping and sequence…

peptide-mapping
peptide-mapping

Enzymatic digestion followed by LC-MS/MS to confirm sequence rather than just mass. The method that catches a scrambled sequence or a D-amino-acid…

103 questions
lc-ms
lc-ms

Liquid chromatography coupled to mass spectrometry: separation and identification in one run, and the method of choice when you need to know not…

10 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
semaglutide
semaglutide

A GLP-1 receptor agonist with a fatty-acid-acylated backbone and a roughly one-week half-life, marketed for type 2 diabetes and for weight…

470 questions
batch-testing
batch-testing

Testing at the batch or lot level: sampling plans, how many vials from a lot need testing to say anything about the lot, and the difference…

910 questions
asked by fiadh_cronin 58k · 12 months ago
22 votes 5 answers4.5k views
What does a 1 Da mass shift on an ESI-MS spectrum indicate?

The method section is present, which is unusual enough that I want to make use of it. I have read the primary source rather than the summary, which has left me with…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
peptide-mapping
peptide-mapping

Enzymatic digestion followed by LC-MS/MS to confirm sequence rather than just mass. The method that catches a scrambled sequence or a D-amino-acid…

103 questions
asked by ivo_paunovic 16k · 2 months ago
21 votes 5 answers9.3k views
How do I compute the +5 charge state m/z for a peptide of 4207.2 Da?

Conditions: +5 · 4207.2 Da. I want the working, not the result — I need to be able to redo it with different numbers. I care about the precision as well as the value…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by petra_hovland 35k · 6 months ago
20 votes 5 answers26k views
What is aspartimide formation and how would I detect it?

I have continuous temperature data for the period in question, which is unusual and I would like to use it. I would like the mechanism, because I want to be able to…

peptide-stability
peptide-stability

The chemistry of peptide degradation: deamidation, oxidation, hydrolysis, aggregation and fibrillation, and how temperature, pH, ionic strength,…

908 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
asked by kirsi_lahtinen 25k · 14 months ago
20 votes 5 answers8.4k views
How do I compute the +3 charge state m/z for a peptide of 4113.6 Da?

What I am working with: +3 · 4113.6 Da. I have worked this out and I would like someone to find the error, because I suspect there is one. My working so far, for the…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by thabo_maseko 28k · 5 months ago
19 votes 5 answers22k views
How do I compute the +2 charge state m/z for a peptide of 4113.6 Da?

Details up front: +2 · 4113.6 Da. I can do the algebra. I am not confident about the conversion factors. If there is a standard way to lay this out, I would rather…

mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
dosing-math
dosing-math

The arithmetic itself: milligrams to millilitres to insulin units, concentration after reconstitution, dose per draw, and vial-days per vial. Show…

764 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
asked by rota_site 36k · 12 months ago
19 votes 5 answers22k views
Would a residual-solvent screen distinguish hydrolysis from a synthesis impurity in ecnoglutide?

The case in front of me: a residual-solvent screen · hydrolysis · ecnoglutide. Both of these get recommended confidently by different people, which suggests neither…

peptide-mapping
peptide-mapping

Enzymatic digestion followed by LC-MS/MS to confirm sequence rather than just mass. The method that catches a scrambled sequence or a D-amino-acid…

103 questions
purity
purity

Purity as chromatographic area per cent - the fraction of detected material that is your target peak. It says nothing about how much material is…

833 questions
mass-spec
mass-spec

Mass spectrometry for identity confirmation: electrospray ionisation, multiple charge states, monoisotopic versus average mass, deconvolution, and…

52 questions
residual-solvent
residual-solvent

Solvents left behind by synthesis and purification - acetonitrile, TFA, DMF, DCM - their ICH limits, how they are measured by headspace GC, and…

14 questions
ecnoglutide
ecnoglutide

A long-acting GLP-1 receptor agonist with a cAMP-biased signalling profile. A niche tag, mostly used for mechanism questions about biased agonism…

223 questions
asked by colm_dunphy 8.2k · 18 months ago
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