
Dushyant Patel LC-MS/MS Method
S.K.P.C.P.E.R., Kherva 37 M .Pharm. Thesis
4.2.8 METHOD DEVELOPMENT TRIALS:
TABLE NO: 4.9 METHOD DEVELOPMENT TRIALS
SR
NO
TRIAL COLUMN MOBILE
PHASE
SAMPLE OBSERVATION
1. TRIAL-1 Betabasic C8,
50 × 4.6 mm,
5 µ
ACN: 10 mM
Amm. formate
( 80:20)
Aqueous
MQC
peak shape was not
good
2. TRIAL-2 Betabasic C8,
50 × 4.6 mm,
5 µ
ACN: 5 mM
Amm. formate
( 80:20)
Aqueous
MQC
IS peak shape was
not good
3. TRIAL-3 Betabasic C8,
50 × 4.6 mm,
5 µ
ACN: 1 mM
Amm. formate
( 80:20)
Aqueous
MQC
peak shape was
good , but higher
tailing observed
4. TRIAL-4 Betabasic C8,
50 × 4.6 mm,
5 µ
ACN: Methanol:
5 mM Amm.
formate
( 60:20:20)
Aqueous
MQC
peak shape was
good , but higher
tailing observed
5. TRIAL-5 Betabasic C8,
50 × 4.6 mm,
5 µ
ACN: Methanol:
1 mM Amm.
formate
( 60:20:20)
Aqueous
MQC
peak shape was
good, but higher
tailing was
observed
6. TRIAL-6 Betabasic C8,
50 × 4.6 mm,
5 µ
ACN: Methanol:
1 mM Amm.
formate
( 40:40:20)
Aqueous
MQC
peak shape was
good, slight higher
tailing was
observed
7. TRIAL-7 Symmetry C8,
150 × 4.6 mm,
5 µ
ACN: Methanol:
1 mM Amm.
formate
( 40:40:20)
Aqueous
MQC
peak shape was
good, slight less
tailing was
observed
8. TRIAL-8 Symmetry C8,
150 × 4.6 mm,
5 µ
Methanol :
1 mM Amm.
formate
( 80:20)
Aqueous
MQC
peak shape was
good, tailing was
not observed
9. TRIAL-9 Symmetry C8,
150 × 4.6 mm,
5 µ
Methanol :
1 mM Amm.
formate
(80:20)
Aqueous
MQC &
External
spiked
MQC
peak shape was
good, ion
suppression was
observed
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