Validation of liquid chromatography mass spectrometry (LC-MS) methods

Self test 2.7

1. LC with MS detection is perhaps the most reliable means for confirmation of analyte‘s identity. Please rank the following identity confirmation situations according to reliability (1 is the most reliable). The directive 2002/657/EC can be used as guidance.
LC retention time (k > 1) and a single MS/MS transition
4

Unselect

1

Unselect

2

Unselect

3

Unselect

LC retention time on two different columns (both have k > 1) and a single MS/MS transition (same transitions for both columns).
4

Unselect

1

Unselect

2

Unselect

3

Unselect

LC retention time (k > 1) and MS/MS with a single precursor ion with two product ions
4

Unselect

1

Unselect

2

Unselect

3

Unselect

LC retention time (k > 1), MS/MS with two transitions, of which one of the product ions is detected with HRMS
4

Unselect

1

Unselect

2

Unselect

3

Unselect

2. HPLC analysis of one analyte in one sample and 5 calibration solutions was carried out.

Assess if the analyte presence in the sample can be confirmed by the retention time criterion set by SANTE.
AnalysisRet. Time of analyte, min
Calibrant 14.298
Calibrant 24.413
Calibrant 34.211
Calibrant 44.368
Calibrant 54.183
Sample4.122

3. HPLC analysis of one analyte in one sample and 5 calibration solutions was carried out.

Assess if the analyte presence in the sample can be confirmed by the retention time criterion set by 2002/675/EC.
AnalysisRet. Time of analyte, minRet. Time of ret.time standard compound, min
Calibrant 14.29811.191
Calibrant 24.41311.24
Calibrant 34.21111.144
Calibrant 44.36811.309
Calibrant 54.18311.195
Sample4.12211.277


 

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