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Beclomethasone Dipropionate

Molecular formula: C28H37CIO7 Molecular weight: 521.1 CAS Registry No.: 5334-09-8 (beclomethasone dipropionate), 4419-39-0 (beclomethasone)

SAMPLE

Matrix: blood Sample preparation: 50 |xL Plasma + 100 jxL 20 |xg/mL cloprednol + 3 mL ether, shake 10 min, centrifuge at 3000 g, remove the organic phase and evaporate it to dryness under nitrogen. Take up the residue in 200 |xL mobile phase, inject a 50 jxL aliquot.
HPLCVARIABLES

Column: Nucleosil R 10 C 18 Mobile phase: MeOH: MeCN: water: acetic acid 400:100:200:1 Injection volume: 50 Detector: UV 254
CHROMATOGRAM

Internal standard: cloprednol Limit of detection: 500 ng/mL


KEYWORDS

plasma
REFERENCE
Wiirthwein, G.; Rohdewald, P. Activation of beclomethasone dipropionate by hydrolysis to beclomethasone-17-monopropionate. Biopharm.Drug Dispos., 1990, 11, 381-394

SAMPLE

Matrix: blood, tissue Sample preparation: Acidify plasma or lung tissue homogenate to pH 2 with 500 mM HCl, add 100 |xL 20 |JLg/mL IS, extract with 8 mL dichloromethane. Evaporate the organic layer to dryness under vacuum, reconstitute in 120 |JLL MeOH: 5% acetic acid 50:50, inject an 80 \xL aliquot.
HPLCVARIABLES

Column: 250 X 4.6 5 |xm Zorbax ODS C18 Mobile phase: MeCN: MeOH: water 44:11:45 Flow rate: 1 Injection volume: 80 Detector: UV 242; Radioactivity
CHROMATOGRAM

Internal standard: hydrocortisone 21-S-propionate (JO 498)


OTHER SUBSTANCES

Extracted: metabolites, budesonide


KEYWORDS

rat; lung; radiolabeled; pharmacokinetics; plasma

REFERENCE
Chanoine, F.; Grenot, C; Heidmann, P.; Junien, J.L. Pharmacokinetics of butixocort 21-propionate, budesonide, and beclomethasone dipropionate in the rat after intratracheal, intravenous, and oral treatments. Drug Metab.Dispos., 1991, 19, 546-553

SAMPLE Matrix: formulations Sample preparation: Ointment. Add pentane:EtOH 75:25 to ointment, sonicate for 20 min, dilute an aliquot to 100 mL with MeOH, allow to settle. Centrifuge and filter an aliquot of the supernatant, inject an aliquot of the nitrate. Cream, lotion. Stir cream or lotion in EtOH: THF: water 25:25:50 at 40 for 15 min, cool in an ice bath. Centrifuge and filter an aliquot of the supernatant, inject an aliquot of the filtrate. Gel. Dissolve gel in EtOH, sonicate, filter, inject an aliquot. HPLCVARIABLES Guard column: present but not specified Column: 250 X 2.1 10 |xm Bondapak C18 Mobile phase: MeCN: water 48:52 containing 0.65% acetic acid, pH 3.18 (At the end of each day flush guard column only with MeOH: THF 75:25 for 30 min.) Flow rate: 1 Injection volume: 20 Detector: UV 251 CHROMATOGRAM Retention time: 8.78 OTHER SUBSTANCES Simultaneous: bamipine lactate, betamethasone-17-valerate, dexamethasone, hydrocortisone-21-acetate KEYWORDS ointment; creams; lotions; gels REFERENCE
Kountourellis, J.E.; Markopoulou, C.K.; Ebete, K.O.; Stratis, J.A. Separation and determination of some corticosteroids combined with bamipine in pharmaceutical formulations by high performance liquid chromatography. J.Liq.Chromatogr., 1995, 18, 3507-3517

SAMPLE Matrix: ileostomy effluent Sample preparation: Dilute ileostomy effluent 1:2 by weight with water and mix with 100 |xL 11 [LgImL 17-hydroxyprogesterone. Extract 3 g aliquot three times with 10 mL dichloromethane by shaking for 1 min and centrifuging at 2000 rpm for 2 min. Wash combined extracts successively with 2 mL 0.1 M NaOH and 4 mL water by shaking for 30 s and centrifuging for 1 min then dry the organic layer under air at 40. Take up the extract in 1 mL MeOH, add 1.1 mL water and apply to C18 Bond Elut SPE cartridge. Wash with 10 mL water, wash with 5 mL MeOH: water 45:55, elute with 2 mL MeOH. Add 50 |xL 20 \xg/mL progesterone to the eluate, dry at 40, take up in 100 |xL MeOH,
inject 10 JJLL aliquot.

HPLC VARIABLES Guard column: Bondapak C18/Corasil Column: 300 X 3.9 ixBondapak C18 Mobile phase: MeOH: 50 mM pH 3.0 sodium phosphate buffer 55:45

Flow rate: 3

Injection volume: 10 Detector: UV 254; UV 238 CHROMATOGRAM Retention time: 21.3 Internal standard: 17-hydroxyprogesterone (6.0), progesterone (11.6) OTHER SUBSTANCES Extracted: beclomethasone alcohol, beclomethasone 17-monopropionate KEYWORDS SPE REFERENCE
Levine, D.S.; Raisys, V.A.; Ainardi, V. Coating of oral beclomethasone dipropionate capsules with cellulose acetate phthalate enhances delivery of topically active antiinflammatory drug to the terminal ileum. Gastroenterology, 1987, 92, 1037-1044

SAMPLE Matrix: solutions HPLC VARIABLES Column: 250 X 4.6 Zorbax SAX Mobile phase: MeOH: buffer 50:50 (Buffer was 180 mM Na2HPO4 adjusted to pH 3.00 0.05 with 180 mM orthophosphoric acid. Pass mobile phase through a 250 X 4.6 25-40 ixm silica (HPLC Technology) column to saturate it with silica.) Flow rate: 1 Detector: UV 253 CHROMATOGRAM Retention time: 2.7 OTHER SUBSTANCES Simultaneous: cromolyn, minocromil, nedocromil, quinoline yellow, saccharin, salicylic acid Interfering: acetaminophen, albuterol, aspartame, aspirin, caffeine, isoproterenol, menthol, reproterol, riboflavin, sorbitan trioleate, terbutaline, theophylline REFERENCE
Baker, P.R.; Gardner, J.J.; Wilkinson, D. Automated high-performance liquid chromatographic method for the determination of nedocromil sodium in human urine using bimodal column switching. J.Chromatogr.B, 1995, 668, 59-65

SAMPLE Matrix: tissue Sample preparation: 100 mg Tissue + 2 mL Ringer's pH 6.8 phosphate buffer + 2 mL EtOH, centrifuge, wash residue twice. Pool supernatant and washings and evaporate to dryness, take up in 400 (JLL EtOH, inject an aliquot. HPLCVARIABLES Guard column: present but not specified Column: ixBondapak C18 Mobile phase: Gradient. MeOH.water 40:60 to 80:20, time not specified Flow rate: 1.5 Detector: UV 254

OTHER SUBSTANCES Extracted: beclomethasone monopropionate, beclomethasone, cyclomethasone KEYWORDS

lung
REFERENCE
Ronca-Testoni, S. Hydrolysis of cyclomethasone by the human lung. Int.J.Clin.Pharmacol.Res., 1983, 3, 17-20

ANNOTATED BIBLIOGRAPHY

Valvo, L.; Paris, A.; Savella, A.L.; Gallinella, B.; Ciranni Signoretti, E. General high-performance liquid chromatographic procedures for the rapid screening of natural and synthetic corticosteroids. J.Pharm.Biomed.AnaL, 1994, 12, 805-810 [gradient; reverse phase; normal phase; also betainethasone, betamethasone 21-acetate, betamethasone 17,21-dipropionate, betamethasone 21-disodium phosphate, betamethasone 17-valerate, cortisone, cortisone 21-acetate, 11-deoxycorticosterone 21acetate, dexamethasone, dexamethasone 21-acetate, dexamethasone 21-disodium phosphate, fluocinolone, fluocinolone acetonide, 9a-fluorohydrocortisone, 9a-fluorohydrocortisone 21-acetate, 9a-fluoroprednisolone, 9a-fluoroprednisolone 21-acetate, hydrocortisone, hydrocortisone 21-acetate, hydrocortisone 21-hemisuccinate, 6a-methylprednisolone, 6a-methylprednisolone 21-acetate, Garnet hylprednisolone 21-sodium succinate, prednisolone, prednisolone 21-acetate, prednisolone 21-disodium phosphate, prednisolone 21-pivalate, prednisolone 21-sodium succinate, prednisone, triamcinolone, triamcinolone acetonide] Girault, J.; Istin, B.; Malgouyat, J.M.; Brisson, A.M.; Fourtillan, J.B. Simultaneous determination of beclomethasone, beclomethasone monopropionate and beclomethasone dipropionate in biological fluids using a particle beam interface for combining liquid chromatography with negative-ion chemical ionization mass spectrometry. J.Chromatogr., 1991, 564, 43-53 [plasma; urine; LC-MS; LOQ 1 ng/mL]

Benazepril
Molecular formula: C24H28N2O5 Molecular weight: 424.5 CAS Registry No.: 86541-75-5 (benazepril), 86541 -74-4 (benazepril hydrochloride)

SAMPLE Matrix: blood Sample preparation: 2 mL Whole blood or plasma + 2 mL buffer + 5 mL chloroform: isopropanol: n-heptane 60:14:26, shake gently horizontally for 10 min, centrifuge at 2800 g for 10 min. Remove the lower organic layer and evaporate it to dryness under vacuum at 45, reconstitute the residue in 100 JJIL mobile phase, centrifuge at 2800 g for 5 min, inject a 50 fxL aliquot of the supernatant. (Buffer was saturated ammonium chloride solution 25% diluted with water, adjusted to pH 9.5 with 25% ammonia solution.) HPLCVARIABLES Column: 300 X 3.9 4 |xm NovaPack C18 Mobile phase: MeOH:THF:buffer 65:5:30 (Buffer was 0.68 g/L (10 mM (sic)) KH2PO4 adjusted to pH 2.6 with concentrated orthophosphoric acid.) (At the end of each session wash the column with water for 1 h and MeOH for 1 h, re-equilibrate for 30 min.) Column temperature: 30 Flow rate: 0.8 Injection volume: 50 Detector: UV 239 CHROMATOGRAM Retention time: 5.01 Limit of detection: <120 ng/mL OTHER SUBSTANCES Extracted: acebutolol, acepromazine, aceprometazine, acetaminophen, aconitine, ajmaline, albuterol, alimemazine, alminoprofen, alpidem, alprazolam, alprenolol, amisulpride, amitriptyline, amodiaquine, amoxapine, aspirin, astemizole, atenolol, benperidol, benzocaine, benzoylecgonine, bepridil, betaxolol, bisoprolol, bromazepam, brompheniramine, bumadizone, bupivacaine, buprenorphine, buspirone, caffeine, carbamazepine, carbinoxamine, carpipramine, carteolol, celiprolol, cetirizine, chlorambucil, chlormezanone, chlorophenacinone, chloroquine, chlorpheniramine, chlorpromazine, chlorpropamide, cibenzoline, cicletanine, clemastine, clobazam, clomipramine, clonazepam, clonidine, clozapine, cocaine, codeine, colchicine, cyamemazine, cyclizine, cycloguanil, cyproheptadine, cytarabine, dacarbazine, daunorubicin, debrisoquine, demexiptiline, desipramine, dextromethorphan, dextromoramide, dextropropoxyphene, diazepam, diazoxide, diclofenac, dihydralazine, diltiazem, diphenhydramine, disopyramide, dosulepine, doxepin, doxylamine, droperidol, ephedrine, estazolam, etodolac, fenfluramine, fenoprofen, fentiazac, flecainide, floctafenine, flumazenil, flunitrazepam, fluoxetine, fluphenazine, flurbiprofen, fluvoxamine, glibenclamide, glibornuride, glipizide, glutethimide, haloperidol, histapyrrodine, hydroxychloroquine, hydroxyzine, ibuprofen, imipramine, indomethacin, iproniazid, ketamine, ketoprofen, labetalol, levomepromazine, lidocaine, lidoflazine, lisinopril, loperamide, loprazolam, loratadine, lorazepam, loxapine, maprotiline, medazepam, medifoxamine, mefenamic acid, mefenidramine, mefloquine, melphalan, meperidine, mephenesin, mephentermine, mepivacaine, metformin, methadone, methaqualone, methocarbamol, methotrexate, metipranolol, metoclopramide, metoprolol, mianserine, midazolam, minoxidil, moclobemide, moperone, morphine, nadolol, nalbuphine, nalorphine, naloxone, naltrexone, naproxen, nialamide, nicardipine, nifedipine, niflumic acid, nimodipine, nitrazepam,

nitrendipine, nizatidine, nortriptyline, omeprazole, opipramol, oxazepam, penbutolol, penfluridol, pentazocine, phencyclidine, phenobarbital, phenol, phenylbutazone, pimozide, pindolol, piroxicam, prazepam, prazosin, prilocaine, procainamide, procarbazine, proguanil, promethazine, propafenone, propranolol, protriptyline, quinidine, quinine, quinupramine, ramipril, ranitidine, reserpine, ritodrine, secobarbital, sotalol, strychnine, sulfinpyrazole, sulindac, sulpride, sultopride, suriclone, temazepam, tenoxicam, terbutaline, terfenadine, tetracaine, tetrazepam, thiopental, thioproperazine, thioridazine, tianeptine, tiapride, tiaprofenic acid, timolol, tioclomarol, tofisopam, tolbutamide, toloxatone, triazolam, trifluoperazine, trifluperidol, trimipramine, triprolidine, tropatenine, verapamil, viloxazine, vinblastine, yohimbine, zolpidem, zopiclone, zorubicine Interfering: acenocoumarol, benazepril, chlordiazepoxide, clorazepate, dipyridamole, metapramine, mexiletine, nomifensine, oxprenolol, pipamperone, pyrimethamine, ticlopidine, trazodone, vincristine, vindesine, warfarin KEYWORDS whole blood; plasma REFERENCE
Tracqui, A.; Kintz, P.; Mangin, P. Systematic toxicological analysis using HPLC/DAD. J.Forensic ScL, 1995, 40, 254-262

SAMPLE Matrix: blood Sample preparation: Condition a Bond-Elut C2 SPE cartridge with 2 mL MeOH and 2 mL water. Adjust pH of plasma to 1.0 with dilute phosphoric acid, add 1 mL to the SPE cartridge, wash with pH 1.0 dilute phosphoric acid, wash with water, wash with EtOH, wash with MeCN, air dry, elute with 200 \xL mobile phase, inject an aliquot. HPLCVARIABLES Guard column: Newguard-Phenyl Column: 150 X 3.9 ixBondapak phenyl Mobile phase: MeOH: water 49:51 with 1 vial PIC-A reagent/L, adjusted to pH 7.0 with phosphoric acid Flow rate: 1 Detector: UV 210 KEYWORDS plasma; dog; SPE; pharmacokinetics REFERENCE
Kim, J.S.; Oberle, R.L.; Krummel, D.A.; Dressman, J.B.; Fleisher, D. Absorption of ACE inhibitors from small intestine and colon. J.Pharm.ScL, 1994, 83, 1350-1356

SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.6 Spherisorh 5 ODS-2 Mobile phase: n-Propanol: buffer 20:80 (Buffer was pH 3.0 phosphate buffer containing 0.4% triethylamine.) Flow rate: 1 Detector: UV 240 CHROMATOGRAM Retention time: 14

OTHER SUBSTANCES Simultaneous: captopril, cilazapril, enalapril, quinapril, ramipril REFERENCE Barbato, F.; Morrica, P.; Quaglia, F. Analysis of ACE inhibitor drugs by high performance liquid chromatography. Farmaco, 1994, 49, 457-460