3mL, Bond Elut Certifi 130mg. PN.12102051
Tricyclic antidepressant solid phase extraction purification method
Sample preparation
A. Plasma or serum
Adjust the pH to 6.0 ± 0.5 1 mL with 1.0 mol/L KOH solution. Add 4 mL of 100 mmol/L phosphate buffer (pH 6.0) and mix thoroughly.
B. Whole blood
Mix well and add 2 mL of methanol to 1 mL of blood. Centrifuging to remove protein precipitates;
Add 10 mL of 100 mmol/L phosphate buffer (pH 6.0, mix well, take the supernatant. Adjust the pH to 6.0 ± 0.5 with 1.0mol/L KOH solution).
2. SPE purification
Flush the column bed with 2 mL of deionized water and 1 mL of 100 mmol/L phosphate buffer (pH 6.0; a. Activation: use 2 mL of methanol.
Note: Make sure the adsorbent is not dry;
b. Loading: The loading flow rate is controlled at 1~2mL/min
1 mL of 1.0 mol/L acetic acid and 3 mL of methanol were separately rinsed, c. Leaching: 3 mL of deionized water, respectively. After the zui, the SPE column is pumped for 5 minutes to dryness;
d. Elution: Elution with 2 mL of dichloromethane/isopropanol/ammonia (78:20:2 at a rate of 1 to 2 mL/min. Collect all eluents;
Note: The eluent must be a freshly prepared fresh solution for the day.
3. Evaporative drying
Rotate the eluent to a temperature below 40 °C
4. Detection method
GC-NPD or GC-MS analysis
derivatization
After reacting at 70 °C for 20 min, cool to room temperature, dissolve the evaporated sample with 50 μL of ethyl acetate, add 50 μL of pentafluoropropionyl anhydride (PFPA is filled with nitrogen and sealed. Evaporate to dryness; 100 μL of ethyl acetate to volume
Derivative method
Re-constant with 100 μL of methanol; 1 to 3 μL; samples without derivatization can be directly analyzed.
LC detection
The sample in step 3 was measured with 200 μL of acetonitrile/deionized water (25:75). Mix 30 to 100 μL with a vortex mixer.
5. Sample composition
Tricyclic antidepressant
Solid phase extraction device used in the method
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