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Analytics · Method validation · continued

Second pass at: LOD and LOQ: definitions people get wrong posts 31–52

This is a continuation of a long topic, addressed by post number rather than by page. Start at post 1.

O
OTeixeiraTL3Regular4 Sep 2025#31

Whatever the answer on LOD and LOQ turns out to be, the method for getting there is the same: state the assumption, do the arithmetic in public, invite the correction.

30 likes 11mo
SO
s.oyelaranTL25 Sep 2025#32
b.correia, post #17: System suitability is the ongoing evidence that a validated method is still performing. Validation is done once; suitability is done every run, and it is the one that appears on a certificate. The general case is well covered; this is the awkward specific one. Go to post

That is the distinction I keep failing to hold on to. Written down now.

15 likes in reply to #17 11mo
CD
cohort_driftTL3Regular5 Sep 2025#33
o.pasquale, post #29: Picking up post #26: that is the part I would want checked first. LOD and LOQ would be much easier to settle if anyone reported the denominator. Almost nobody reports the denominator. Go to post

Reading this LOD and LOQ thread as someone who came in with a fixed view: the third and seventh replies moved me and the confident ones did not.

3 likes in reply to #29 11mo
IO
i.oseiTL26 Sep 2025#34

The arithmetic in post #31 is right; the assumption feeding it is the part to check.

System suitability is the ongoing evidence that a validated method is still performing. Validation is done once; suitability is done every run, and it is the one that appears on a certificate.

0 likes 11mo
EM
endpoint_marginTL2Member6 Sep 2025#35

Post #31 put the caveat in the right place and I want to underline it.

LOD and LOQ was covered in the wiki last year and the page has a review date on it, which is a better starting point than my memory of a thread.

22 likes 11mo
BT
b.teixeiraTL27 Sep 2025#36
IMainwaring, post #4: Where the LOD and LOQ discussion usually stalls is that nobody wants to say "I do not know" and everyone is willing to say "it varies". Those are the same sentence with different clothes on. Go to post

Filing a mild objection to the consensus on LOD and LOQ. Mild because I might be wrong; an objection because nobody has addressed the case that does not fit.

10 likes in reply to #4 11mo
M
MJayawardenaTL3Regular7 Sep 2025#37

The most useful single question about a method: what would it fail to detect? Every method has an answer and few documents state it.

A qualification I should have led with rather than closed on.

1 like 11mo
RC
r.coelhoTL28 Sep 2025 · edited#38

A definition problem is doing most of the work in this LOD and LOQ discussion. Once the term is pinned down I suspect the disagreement mostly goes away and what is left is small.

0 likes 11mo
AS
a.salcedoTL3Regular9 Sep 2025#39
MJayawardena, post #37: The most useful single question about a method: what would it fail to detect? Every method has an answer and few documents state it. A qualification I should have led with rather than closed on. Go to post

Quietly grateful for the plain phrasing. Not every thread gets that.

16 likes in reply to #37 11mo
KH
ka.haddadTL29 Sep 2025#40
o.pasquale, post #29: Picking up post #26: that is the part I would want checked first. LOD and LOQ would be much easier to settle if anyone reported the denominator. Almost nobody reports the denominator. Go to post

Taking post #38 at face value and following it one step further.

Practical experience of LOD and LOQ, offered as one case with the conditions stated, not as a general finding. Conditions first, because they are what make it interpretable.

6 likes in reply to #29 11mo
JI
j.iyerTL210 Sep 2025#41

The limit of quantitation determines what the impurity table can honestly contain. Peaks below it can be reported as detected and cannot be reported as a number.

That has held every time I have looked, which is not the same as always.

0 likes 11mo
B
batchlogTL310 Sep 2025#42
SK
s.kuuselaTL211 Sep 2025 · edited#43

The arithmetic in post #40 is right; the assumption feeding it is the part to check.

Offering a way to settle LOD and LOQ rather than another opinion about it. Two measurements, taken the same way, a fortnight apart. If the difference is within the noise, the question was not answerable at this precision.

10 likes 11mo
TY
two_year_lineTL3Regular11 Sep 2025#44

Answering the question post #43 raises rather than the one it answers.

Second-hand on LOD and LOQ, so weight it accordingly — someone whose method I trust told me this and I have not verified it myself.

22 likes 11mo
GR
g.radichTL212 Sep 2025#45

Building on post #44 rather than restating it.

The most useful single question about a method: what would it fail to detect? Every method has an answer and few documents state it.

0 likes 10mo
MM
maintenance_modeTL3Regular12 Sep 2025#46
s.ivaturi, post #28: I would rather this thread reach "we do not know" about LOD and LOQ than reach a confident answer that nobody can support when asked. Go to post

The bit of LOD and LOQ that nobody enjoys is that the answer changes depending on what you are trying to decide with it. Say what the decision is and the thread will converge.

1 like in reply to #28 10mo
KP
k.pereiraTL213 Sep 2025#47

Worth stating the null on LOD and LOQ before we explain it: the observation may be nothing. That possibility deserves a sentence and usually does not get one.

6 likes 10mo
RV
r.venkatesanTL3Wiki editor13 Sep 2025#48

Everything in post #46 holds. The case it does not cover is the one I have.

Why two laboratories may disagree: after validating the same method, they may still report different purity on the same sample due to integration differences, column age differences, subtle differences in mobile phase pH or temperature. This is normal and not a sign that one is wrong.

16 likes 10mo
HB
h.brandtTL214 Sep 2025#49

Post #48 is right about the mechanism and I think understates the practical bit.

The claim about LOD and LOQ upthread is stronger than its source supports. I have read the source. The source says "associated with" and the post says "causes".

2 likes 10mo
IS
isotonic_sheetTL3Regular14 Sep 2025 · edited#50

Coming back to post #46, because the follow-up matters more than the original answer.

My understanding of LOD and LOQ is a few years old and may have been superseded. If it has been, I would genuinely like to know rather than keep repeating it.

9 likes 10mo
NS
n.serranoTL215 Sep 2025#51

Where a pharmacopoeial monograph exists, a method that follows it inherits a great deal of assurance. Almost nothing discussed here has one.

Scoping that to what I have actually seen rather than what I have read.

0 likes 10mo
RM
r.marsdenTL3Regular15 Sep 2025#52
vial_slope, post #8: Helpful, and short, which on this subject is harder than long. Go to post

Precision has two levels worth distinguishing: repeatability within a run and intermediate precision across days, analysts and instruments. The second is where most methods lose the numbers people quote.

Happy to expand any of that if it is the useful part.

21 likes in reply to #8 10mo

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