Indapamide

Molecular formula: C16H16CIN3O3S Molecular weight: 365.8 CAS Registry No.: 26807-65-8

SAMPLE Matrix: blood Sample preparation: 1 mL Whole blood + 1 mL 4 jmg/mL glipizide in 50 mM pH 6.6 KH2PO4, vortex, add 6 mL diethyl ether, shake at 150 20 oscillations/min on a reciprocating shaker for 15 min, centrifuge at 1500 g for 10 min. Remove the organic layer and evaporate it to dryness at 37 under a stream of nitrogen. Dissolve residue in 200 JJIL mobile phase, centrifuge at 1000 g for 3 min, inject a 40 |xL aliquot of the supernatant. HPLCVARIABLES Column: 150 x 4.6 5 |xm Nucleosil C18 Mobile phase: MeCN:isopropanol:buffer 30:5:65 (Buffer was 80 mM ammonium acetate adjusted to pH 3.5 with concentrated HCl.) Flow rate: 1 Injection volume: 40 Detector: UV 241 CHROMATOGRAM Retention time: 5.2 Internal standard: glipizide (5.9) Limit of quantitation: 10 ng/mL OTHER SUBSTANCES Noninterfering: acetaminophen, aspirin, caffeine, dextromethorphan, ibuprofen, nicotine, phenylpropanolamine, theophylline KEYWORDS whole blood REFERENCE
Miller, R.B.; Dadgar, D.; Lalande, M. High-performance liquid chromatographic method for the determination of indapamide in human whole blood. J.Chromatogr., 1993, 614, 293-298

SAMPLE Matrix: blood Sample preparation: Condition a Sep-Pak C18 SPE cartridge with 5 mL MeOH and 5 mL 10 mM HCl. 2 mL Plasma + 2 mL 2 |ig/mL IS in water + 10 mL 10 mM HCl, add to the SPE cartridge, wash with 4 mL 10 mM HCl, elute with 1 mL MeOH, inject a 20 \xL aliquot of the eluate. HPLCVARIABLES Column: 250 X 4 10 [xm LiChrosorb SI 60 ODS Mobile phase: MeCN: 10 mM pH 3.5 sodium phosphate 30:70 Flow rate: 1 Injection volume: 20 Detector: UV 241 CHROMATOGRAM Retention time: 9

Internal standard: sulfadimethoxime (6.2) Limit of detection: 10 ng/mL KEYWORDS plasma; SPE; see Anal.Abs. 1986, 48, 12D80 REFERENCE
Gaetani, E.; Laureri, CR; Vitto, M.; Borghi, L.; Elia, G.F.; Novarini, A. Determinazione deirindapamide nel plasma mediante HPLC [Determination of indapamide in plasma by HPLC]. Boll.Chim.Farm., 1986, 125, 35-37

SAMPLE Matrix: blood Sample preparation: Keep tubes in crushed ice except when being processed throughout this procedure. 2 mL Plasma + 100 jxL 10 |xg/mL sulfanilamide in MeCN + 8 mL diethyl ether, vortex for 2 min, centrifuge at 4. Remove ether layer and add it to 1 mL 100 mM NaOH, vortex for 2 min, centrifuge at 4. Remove aqueous layer and add it to 1 mL 100 mM HCl and 500 jxL 50 mM pH 7.4 sodium phosphate, add 8 mL ether, vortex for 2 min, centrifuge at 4. Evaporate ether layer to dryness, reconstitute in 200 |xL mobile phase, inject 50 fxL aliquot. HPLCVARIABLES Column: 250 X 4.6 5 jxm Zorbax ODS Mobile phase: MeCN: 100 mM pH 3.6 sodium acetate buffer 43:57 Column temperature: 54 Flow rate: 1 Injection volume: 50 Detector: UV 241 CHROMATOGRAM Retention time: 6.3 Internal standard: sulfanilamide (5.3) Limit of detection: 25 ng/mL KEYWORDS plasma REFERENCE
Choi, R.L.; Rosenberg, M.; Grebow, RE.; Huntley, T.E. High-performance liquid chromatographic analysis of indapamide (RHC 2555) in urine, plasma and blood. J.Chromatogr., 1982, 230, 181-187

SAMPLE Matrix: bulk, formulations, urine Sample preparation: Bulk, tablets. Weigh out amount containing 10 mg indapamide, dissolve in 10 mL 150 ixg/mL sulfisoxazole in MeOH, make up to 100 mL with MeOH, inject an aliquot. Urine. 1 mL Urine + 1 mL 150 |xg/mL sulfisoxazole in MeOH H - 10 mL ethyl acetate, vortex, centrifuge. Remove the organic layer and evaporate it to dryness under a stream of nitrogen, reconstitute the residue in 1 mL mobile phase, inject a 10 |xL aliquot. (If indapamide concentration is >100 ng/mL mix 1 mL urine, 1 mL 150 |xg/mL sulfisoxazole in MeOH, and 8 mL mobile phase, vortex, inject a 10 JJLL aliquot.) HPLCVARIABLES Guard column: 20 X 4 Bondapak C18 Corasil Column: 300 X 4 10 |xm jxBondapak C18 Mobile phase: MeCN:buffer 35:65 (Buffer was water adjusted to pH 2.8 with 10% phosphoric acid.)

Flow rate: 2 Injection volume: 10 Detector: UV 254 CHROMATOGRAM Retention time: 7 Internal standard: sulfisoxazole (4) Limit of detection: 25 ng/mL OTHER SUBSTANCES Extracted: metabolites KEYWORDS tablets REFERENCE
Pietta, P.; Calatroni, A.; Rava, A. High-performance liquid chromatographic assay for monitoring indapamide and its major metabolite in urine. J.Chromatogr., 1982, 228, 377-381

SAMPLE Matrix: solutions HPLC VARIABLES Column: Chiralcel OD-R Mobile phase: MeCN: water 40:60 Column temperature: 40 Flow rate: 1 Detector: UV 254 CHROMATOGRAM Retention time: 11.3, 15.8 (enantiomers) KEYWORDS chiral REFERENCE
Application Guide for Chiral Column Selection, Second Edition, Chiral Technologies Inc., Exton PA, 1995, p. 39

SAMPLE Matrix: solutions HPLCVARIABLES Column: 250 X 4.6 Chirex 3022 (Phenomenex) Mobile phase: Hexane: 1,2-dichloroethane: EtOH/trifluoroacetic trifluoroacetic acid was premixed 20:1.) Flow rate: 0.7-1 Injection volume: 20 Detector: UV 248 KEYWORDS chiral; a = 1.08 REFERENCE
Cleveland, T. Pirkle-concept chiral stationary phases for the HPLC separation of pharmaceutical racemates. J.Liq.Chromatogr., 1995, 18, 649-671

acid 58:35:7 (EtOH/

SAMPLE Matrix: solutions Sample preparation: Inject a 20 J U L L aliquot. HPLCVARIABLES Column: 250 X 4.6 5 |xm Lichrosorb RP-18 Mobile phase: MeOH.buffer 50:50 (Buffer was 1% aqueous acetic acid containing 0.2% triethylamine.) Flow rate: 1 Injection volume: 20 Detector: UV 250 CHROMATOGRAM Retention time: 11 Limit of detection: 500 ng/mL OTHER SUBSTANCES Simultaneous: degradation products KEYWORDS stability-indicating REFERENCE
Padval, M.V.; Bhargava, H.N. Liquid chromatographic determination of indapamide in the presence of its degradation products. J.Pharm.Biomed.Anal, 1993, 11, 1033-1036

ANNOTATED BIBLIOGRAPHY

Chen, D. [Determination of indapamide in human serum by high performance liquid chromatography]. Chung Kuo I Hsueh Ko Hsueh Yuan Hsueh Pao, 1990, 12, 286-289