Laboratory Procedure Reference
Sample
Preparation
Seven-Category Drug Sample Preparation Guide
7Categories
Anticholesterol · Antidiabetic · Diuretic · PPI · Antihypertensive · EDD · DomperidoneDrug Classes
Syarief AzmanPrepared by
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OverviewAnticholesterol — Sample Preparation
Including Capsule Shells
Solvent: MeOH
50 mL Centrifuge Tube
Centrifuge: 1 g sample in 50 mL centrifuge tube → 20 mL MeOH → sonicate 15 min at 37°C → centrifuge 4000 rpm × 5 min → filter into 2 mL amber vial.
ProcedureStep-by-Step — tap each step to check off
01
Weigh
Weight 1 g of the sample (including capsule shells) into a 50 mL centrifuge tube
02
Dissolve & Sonicate
Add in 20 mL of Methanol and sonicate for 15 minutes at 37°C
03
Centrifuge
Centrifuge at 4000 rpm for 5 minutes
⚙ 4000 rpm
04
Filter
Filter the supernatant layer into a 2 mL amber vial using 0.45 μm syringe filter
★ Collect
05
Ready
Sample ready for HPLC injection
✓ Done
OverviewAntidiabetic — Sample Preparation
Tablet Form
Solvent: MeOH
Beaker
**Antidiabetic = Diuretic method variant. Same solvent, different centrifuge speed (3500 rpm) and longer sonicate time (30 min).
ProcedureStep-by-Step
01
Weigh
Weight 1 g of the sample (tablet) in a beaker
02
Dissolve
Dissolve with 20 mL methanol
03
Sonicate
Sonicate the solution for 30 minutes
04
Centrifuge
Centrifuge at 3500 rpm for 15 minutes
⚙ 3500 rpm
05
Filter
Filter supernatant with 0.45 μm syringe filter into 2 mL vial
★ Collect
OverviewDiuretic — Sample Preparation
Including Capsule Shell
Solvent: MeOH
Beaker
Weigh 1.0 g sample (including capsule shell). Use Chloroform/softcapsule not dissolve in MeOH.
ProcedureStep-by-Step
01
Weigh
Weigh 1.0 g of the sample (including capsule shell) in a beaker
02
Dissolve
Dissolve with 20 mL methanol
03
Sonicate
Sonicate the solution for 30 minutes. Use Chloroform if softcapsule — not dissolve in MeOH
⚠ Note
04
Centrifuge
Centrifuge at 3500 rpm for 15 minutes
⚙ 3500 rpm
05
Filter
Filter the supernatant layer with 0.45 μm syringe filter into 2 mL vial
★ Collect
OverviewPPI (Proton Pump Inhibitor) — Sample Preparation
Including Capsule Shells
Solvent: MeOH
50 mL Centrifuge Tube
Two-stage centrifuge process: first at 3500 rpm × 15 min, then at 4500 rpm × 15 min. Filter into amber vial using 0.45 μm syringe filter.
ProcedureStep-by-Step
01
Weigh
Weight 1.0 g of the sample (including capsule shells) into a 50 mL centrifuge tube
02
Dissolve & Sonicate
Add in 20 mL of Methanol and sonicate for 30 minutes
03
Centrifuge — Stage 1
Centrifuge at 3500 rpm for 15 minutes
⚙ 3500 rpm
04
Centrifuge — Stage 2
Centrifuge at 4500 rpm for 15 minutes
⚙ 4500 rpm
05
Filter
Filter the sample solution into the amber vial using 0.45 μm syringe filter
★ Collect
OverviewAntihypertensive — Sample Preparation
Including Capsule Shells
Solvent: MeOH
50 mL Centrifuge Tube
ProcedureStep-by-Step
01
Weigh
Weight 0.5 g of the sample (including capsule shells) into a 50 mL centrifuge tube
02
Dissolve & Sonicate
Add in 20 mL of Methanol and sonicate for 30 minutes
03
Centrifuge
Centrifuge at 4500 rpm for 15 minutes
⚙ 4500 rpm
04
Filter
Filter the sample solution into the amber vial using 0.45 μm syringe filter
★ Collect
05
Ready
Sample ready for HPLC injection
✓ Done
OverviewEDD — Sample Preparation
Powder Form
Solvent: Deionised Water
CHCl₃ Extraction
pH Adjustment Required
Uses Chloroform for extraction — perform all CHCl₃ steps in or near the fume cupboard. Requires pH adjustment to >pH 11 with Ammonium.
ProcedureStep-by-Step
01
Weigh
Weigh 1.5 g of the sample (powder) in a beaker and add 20 mL of deionised water
02
Sonicate
Sonicate for 15 minutes
03
Adjust pH
Adjust the pH of the sample solution to more than pH 11 with Ammonium
⚠ pH > 11
04
Extract
Extract twice with about 50 mL Chloroform
☠ Fume Hood
05
Filter & Combine
Filter the Chloroform layer using 1PS filter paper
★ Collect
06
Evaporate
Combine the Chloroform layer in evaporating dish and evaporate to dryness
☠ Fume Hood
OverviewDomperidone — Sample Preparation
Liquid Sample
Solvent: MeOH
Syringe Filter
Simple liquid preparation: measure sample, transfer to beaker, add methanol → sonicate → filter via 0.45 μm syringe filter.
ProcedureStep-by-Step
01
Measure
Measure 10 mL of the sample (liquid) and transfer to a beaker and add 10 mL of methanol
02
Sonicate
Sonicate for 10 minutes
03
Filter
Filter the sample solution into the vial using 0.45 μm syringe filter
★ Collect