291
(70 eV), ion source temperature 230 °C, scan range m/z
50–800 (positive mode), and interface temperature 280 °C.
2. Internal standards: 2,4-Dihydroxybenzophenone (10 μg/g
solution in isopropanol), internal standard for derivatization
(IS1); hexadecane (100 μg/g solution in iso-octane), internal
standard for injection (IS2).
3. Derivatization agent: N,O-bis(trimethylsilyl)trifluoroacetamide
(BSTFA) containing 1% trimethylchlorosilane. Derivatization
takes place in ethyl acetate (AcOEt).
1. Eluents for HPLC: Water (eluent A) and acetonitrile (eluent
B), both HPLC grade. Mobile-phase modifier: Trifluoroacetic
acid (TFA) 0.1% in both eluents, or formic acid (FA) 0.1–1% in
both eluents.
2. Gradient for HPLC: Starting with 85–90% eluent A, hold for
2–5 min, then increase %B until 90–100% with a linear
gradient.
3. Flow rate: 0.2–1 mL/min, depending on the dimensions of the
column and of the stationary-phase particle diameter.
4. DAD: Acquisition in the 200–650 nm range.
5. Injection volume: 5–20 μL.
1. Eluents for HPLC: Water (eluent A) and acetonitrile (eluent
B), both LC-MS grade. Mobile-phase modifier: Formic acid
(FA) 0.1–1% in both eluents.
2. Gradient for HPLC: Starting with 85–90% eluent A, hold for
2–5 min, then increase %B until 90–100% with a linear
gradient.
3. Flow rate: 0.2–0.4 mL/min, depending on the dimensions of
the column and of the stationary-phase particle diameter.
4. MS and tandem MS: Ionization in electrospray ion source in
negative mode, acquisition in the 100–1700 m/z range by a
ToF analyzer for both MS and tandem acquisitions. Application
of 30–50 V in the collision cell for the collision-induced
dissociation.
5. Injection volume: 1–5 μL.
3 Methods
1. Insert the solution of the supporting electrolyte (0.1 M KCl or
BRB buffer) into the electrochemical cell, and in the salt bridge
of the reference electrode.
2.6 HPLC-DAD
Chromatography
2.7 HPLC-MS/MS
Chromatography
3.1 Cyclic
Voltammetry
Electrochemistry Investigation of Drugs Encapsulated in Cyclodextrins
(70 eV), ion source temperature 230 °C, scan range m/z
50–800 (positive mode), and interface temperature 280 °C.
2. Internal standards: 2,4-Dihydroxybenzophenone (10 μg/g
solution in isopropanol), internal standard for derivatization
(IS1); hexadecane (100 μg/g solution in iso-octane), internal
standard for injection (IS2).
3. Derivatization agent: N,O-bis(trimethylsilyl)trifluoroacetamide
(BSTFA) containing 1% trimethylchlorosilane. Derivatization
takes place in ethyl acetate (AcOEt).
1. Eluents for HPLC: Water (eluent A) and acetonitrile (eluent
B), both HPLC grade. Mobile-phase modifier: Trifluoroacetic
acid (TFA) 0.1% in both eluents, or formic acid (FA) 0.1–1% in
both eluents.
2. Gradient for HPLC: Starting with 85–90% eluent A, hold for
2–5 min, then increase %B until 90–100% with a linear
gradient.
3. Flow rate: 0.2–1 mL/min, depending on the dimensions of the
column and of the stationary-phase particle diameter.
4. DAD: Acquisition in the 200–650 nm range.
5. Injection volume: 5–20 μL.
1. Eluents for HPLC: Water (eluent A) and acetonitrile (eluent
B), both LC-MS grade. Mobile-phase modifier: Formic acid
(FA) 0.1–1% in both eluents.
2. Gradient for HPLC: Starting with 85–90% eluent A, hold for
2–5 min, then increase %B until 90–100% with a linear
gradient.
3. Flow rate: 0.2–0.4 mL/min, depending on the dimensions of
the column and of the stationary-phase particle diameter.
4. MS and tandem MS: Ionization in electrospray ion source in
negative mode, acquisition in the 100–1700 m/z range by a
ToF analyzer for both MS and tandem acquisitions. Application
of 30–50 V in the collision cell for the collision-induced
dissociation.
5. Injection volume: 1–5 μL.
3 Methods
1. Insert the solution of the supporting electrolyte (0.1 M KCl or
BRB buffer) into the electrochemical cell, and in the salt bridge
of the reference electrode.
2.6 HPLC-DAD
Chromatography
2.7 HPLC-MS/MS
Chromatography
3.1 Cyclic
Voltammetry
Electrochemistry Investigation of Drugs Encapsulated in Cyclodextrins