8/20/2019 Midazolam 1 http://slidepdf.com/reader/full/midazolam-1 1/6 SAMPLE Matrix: aqueous humor, blood, tissue, urine Sample preparation: Homogenize tissue 1:2 (w/v). 1 mL Sample + 100 |xL 10 img/mL methaqualone + 1 mL ammonium chloride/ammonium hydroxide buffer (pH 9.2) + 3 mL n-butyl chloride, mix, centrifuge. Remove the organic layer and evaporate it to dryness under nitrogen at 45°, reconstitute the residue with 50 |xL mobile phase, inject a 20 |xL aliquot. HPLCVARIABLES Column: 100 X 8 10 |xm ixBondapak C18 Mobile phase: MeCN: buffer 40:60, pH 3.3 (Buffer was 150 mL 100 mM KH 2 PO 4 made up to 1 L, pH adjusted to 3.3 with 100 mM phosphoric acid.) Flow rate: 2.5 Injection volume: 20 Detector: UV 220 CHROMATOGRAM Retention time: 3.93 Internal standard: methaqualone (6.42) KEYWORDS plasma; liver; kidney REFERENCE Ferslew, K.E.; Hagardorn, A.N.; McCormick, W.F. Postmortem determination of the biological distri- bution of sufentanil and midazolam after an acute intoxication. J.Forensic Sci., 1989, 34, 249—257 SAMPLE Matrix: blood Sample preparation: Condition a Sep-Pak C18 SPE cartridge with water, MeOH, and 100 mM ammonium acetate. 5 mL Plasma + 250 ng detomidine, add to the SPE cartridge, wash with 100 mM ammonium acetate, elute with MeOH: 100 mM ammonium acetate 75:25. Evaporate the eluate to dryness under reduced pressure, reconstitute the residue in 200 |xL mobile phase, inject a 50 |xL aliquot. HPLCVARIABLES Column: 150 X 4.6 5 |xm Hitachi gel Mobile phase: 3056 Mobile phase: MeOH: 100 mM ammonium acetate 65:35 Flow rate: 1 Injection volume: 50 Detector: MS, Hitachi M-1000, APCI interface, drift voltage 21 V, nebulizer 260°, vaporizer 399°, multiplier voltage 1500 VF, m/z 326 Midazolam Molecular formula: C 18 H 13 CIFN 3 Molecular weight: 325.8 CAS Registry No : 59467-70-8 midazolam), 59467-96-8 midazolam hydrochloride), 59467-94-6 midazolam maleate)
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8/20/2019 Midazolam 1
http://slidepdf.com/reader/full/midazolam-1 1/6
SAMPLE
Matrix: aqueous humor, blood, tissue, urine
Sample preparat ion:
Hom ogenize ti ss ue 1:2 (w/v). 1 mL Sam ple + 100 |xL 10 img/mL
m ethaq ualon e + 1 mL amm onium chloride/amm onium hy droxide buffer (pH 9.2) + 3 mL
n-butyl chloride, mix, centrifuge. Remove the organic layer and evaporate it to dryness
under nitrogen at 45°, reconstitute the residue with 50 |xL mobile phase, inject a 20 |xL
aliquot.
HPLCVARIABLES
Column: 100 X 8 10 |xm ixBondapak C18
Mobile phase:
M eC N: buffer 40 :60 , pH 3.3 (Buffer w as 150 mL 100 mM K H
2
PO
4
made up
to 1 L, pH adjusted to 3.3 with 100 mM phosphoric acid.)
Flow ra te:
2.5
Inject ion volume:
20
Detector: UV
220
CHROMATOGRAM
Retent ion t ime: 3.93
Internal s tandard:
methaqualone (6.42)
KEYWORDS
plasma; liver; kidney
REFERENCE
Ferslew, K.E.; Hagardorn, A.N.; McCormick, W.F. Postmortem determination of the biological distri-
bution of sufentanil and midazolam after an acute intoxication. J.Forensic Sci., 1989, 34, 249—257
SAMPLE
Matrix:
blood
Sample preparat ion:
Condition a Sep-Pak C18 SPE cartridge with water, MeOH, and 100
mM ammonium acetate. 5 mL Plasma + 250 ng detomidine, add to the SPE cartridge,
wash with 100 mM am mon ium acetate, elute with MeO H: 100 mM am monium acetate
75:25. Evaporate the eluate to dryness under reduced pressure, reconstitute the residue
in 200 |xL mobile phase, inject a 50 |xL aliquot.
HPLCVARIABLES
Column:
150 X 4.6 5 |xm Hitachi gel
Mobile phase: 3056
Mobile phase:
MeO H: 100 mM am monium acetate 6 5:35
Flow rate: 1
Inject ion volume: 50
Detector:
M S, H itach i M-1000, APC I interface, drift voltage 21 V, neb ulizer 260°, vapo rizer
399°, multiplier voltage 1500 VF, m/z 326
Midazolam
Molecular formula: C
18
H
13
CIFN
3
Molecular weight: 325.8
CAS Registry No : 59467-70-8 midazolam), 59467-96-8 midazolam