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w wz 15«1y Kor. J. Clin. Pharm., Vol. 15, No. 1. 2005 r v p e z n z kw w sƒ { Á½ x Á Á Á Á½x» Á«k Á Á«Ÿ û w w w w t t d w w w w x w yw sƒ Effect of Food on Pharmacokinetics and Pharmacodynamics of Fenofibric Acid after a Single Oral Dose of Fenofibrate Sustained-Release Capsule Hwi-yeol Yun 1, Joung-hyun Kim 1, Eun Joo Lee 1, Soo Youn Chung 2, Sun-oK Choi 2 Hyung Kee Kim 3, Jun-tack Kwon 3, Wonku Kang 4, Kwang-il Kwon 1 1 College of pharmacy, Chungnam National University, Daejeon, 305-764, Korea 2 National Institute of Toxicological Research, Seoul, Korea 3 College of Medicine, Soonchunhyang University, Chunan, Choongnam, Korea 4 Korea Institute of Toxicology, Daejeon, Korea We examined the effects of food on pharmacokinetic and pharmacodynamic properties of fenofibrate released from sustained-release (SR) capsule as therapy for hypolipidemia. Twenty-four healthy volunteers were used in 3 3 crossover pharmacokinetic and pharmacodynamic study; Additional six volunteers were used as a control group(i.e., no fenofibrate administration). A single dose of fenofibrate (SR capsule, 250 mg) was administered on three occasions: after overnight fasting, after consumption of a standard breakfast, and after a high-fat breakfast. Serial blood samples were collected for the next 72 hours. Plasma fenofibric acid concentrations were measured by high performance liquid chromatography, and pharmacokinetic parameters were calculated using ADAPT II program. Plsama triglyceride concentrations were measured by blood chemistry analyzer (CH-100). The pharmacokinetic parameters were significantly affected by food intake. The high-fat breakfast affected the rate of absorption of fenofibrate more than did the standard breakfast and fasted conditions. Plasma concentrations of triglyceride at 24 hours decreased significantly after the administration of fenofibrate compared with the concentration at 0 hours(p<0.05). In healthy volunteers, the bioavailability of fenofibrate was greater when administered via sustained-release capsules immediately after the consumption of food than after fasting condition. Key words G fenofibrate, pharmacokinetic, pharmacodynamic Fenofibrate yw 2-[4-(4-chlorobenzyl)phenoxy]-2- methyl-2-propanoic acid š x e 1) fenofibrate y x fenofibric acid (Fig. 1). Fenofibric acid lipase y yw very low density lipoprotein(vldl)-triglyceride y wš acetyl coenzyme A carboxylase y w w w. w y x x š LDL š x Correspondence to : «Ÿ, PhD û w w w w Ÿ ª 220 û w w w 405y Tel: 042-821-5937, Fax: 042-823-6781 E-mail: kwon@cnu.ac.kr w acetyl coenzyme A w. 2) cholesterol transferase y w sü l y g l k. Fenofibrate peroxisome proliferators activated receptors ã (PPARã) w apolipoprotein C-III wš apolipoprotein ƒ w, chylomicron VLDL ƒw. 3-5) š x q» y x fibrinogen w k. 6) Fenofibrate w z w, g l triglyceride eƒ fenofibrate w w š, w ùk ü. w x 7) fenofibric acid w 34

r v p e 1z n z kw w sƒ 35 cholesterol e w š x z ƒ. 8) š x e Ÿ w š fenofibrate e œ š w w 1z n w z x ƒ z e w Á mwš w. x»» x x r e ( y: 04003, z» : 2007 6 24 ) fenofibrate 250mg w w. x d w» w HPLC k, m p, n-hexane, ethylacetate»k p 1 w.»» HPLC rv(lc-10avp, SHIMADZU Co., Kyoto, Japan),»(SPD10-Avp, SHIMADZU Co., Kyoto, Japan), f (Superspher 100 RP-18, 250 4 mm, I.D. Merck, Germany) w x v w. x triglyceride d w» w Triglyceride liquicolor (Stanbio laboratory INC., Houston, U.S.A) w š, d»» CH-100 (SEAC, Firenze, Italy) w. vx w w w w ww w. ü t t š w w x» w ü,»,», y»» w x yw x»k y w w ù w 2ƒ w 24, x n w x w vx 8 ƒƒ w. vx w z x ƒw. vx û 13 11 š s³ 62.83 ± 8.73 kg, s³ 169.63 ± 7.71 cm, š s³ 21.0 ± 1.64. x n w x w 8 s³ 60.75 ± 5.42 kg, s³ 168.21 ± 8.45 cm, š s³ 20.5 ± 2.23. w n 10 x» ƒš k w w x 3 l fv g er w wš w w. x n p 24 ù 3z w š {» 5 w. r e ƒ 1 e 240 ml wì œ k, t w k, š w k 3 n w š x w. x 3 Table 1. 9) œ r e n w z x w x w. x n w x n n z 1, 2, 3, 4, 5, 6, 7, 9, 12, 24, 48, 72 w 13z ww. x n w Table 1. Meal compositions Standard meal High-fat meal Food Ingredients (g) Food Ingredients (g) Steamed rice Rice (90 g) Steamed rice Rice (90 g) Dried shrimp and sea mustard soup Shrimp dried (20g), Sea mustard dried (5 g) Beef and sea mustard soup Sea mustard dried (6 g), beef brisket (30 g) Grilled yellow croaker Yellow croaker Fried yellow Yellow croaker (70g), (70g) croaker soybean oil (5 g) Whole egg (50 g), Egg roll Whole egg (50 g), Steamed egg Composition sesame oil (1 g) soybean oil (3 g) Boiled Spinach (70 g), Radish salad Korean radish (70g) with soy sauce spinach sesame oil (1 g), seasoned soybean oil (1 g) Kimchi 60 g Kimchi 60 g Apple 100 g Cracker with peanuts 32 g kcal (content of fat, %) 686.3 kcal (19.9%) 908.0 kcal (35.5%) Carbohydrate:Protein:Fat 56.3:23.9:19.9 45.5:19.0:35.5

36 Kor. J. Clin. Pharm., Vol. 15, No. 1, 2005 x n n z 1, 2, 3, 4, 6, 8, 12, 24 w 9z ww. x x xq p x š w k 3000rpm 10 w š x x ¾ -20 o C þ w. x GFOPGJCSJDBDJE Fenofibrate ƒ w fenofibric acid. x fenofibrate, fenofibric acid mw x w. Fenofibric acid t t m p 1 mg/ml z þ jš, m p w 10 ƒ x 100uL ƒw z œx 900uL ƒw fenofibric acid x ƒ ƒƒ 0.1, 0.5, 1, 5, 10, 15 µg/ml ƒ x. t x 1mL y wš m p 50uL, 1 mg/ml clofibric acid (internal standard) 50 ul, 1M HCl 1 ml, n-hexane: ethylacetate(90:10, v/v) 5mL ƒw 20 w z 3000 rpm 10 w.» d w» w, š k z m p : (3:7, v/v) 1mL jš 60 vortexing w w z 5uL w HPLC w. 0.02M (ph 3.4): m p 55: 45 w. 1.0 ml/min,» q 287nm. 10) HPLC j m l fenofibric acid vj ü t w clofibric acid vj w š w x fenofibric acid w. x USJHMZDFSJEF 1 1z n w x triglyceride n 0, 1, 2, 3, 4, 5, 6, 7, 9, 12, 24 ¾ d w š, x n w 0, 1, 2, 3, 4, 6, 8, 12, 24 d w. Triglyceride liqucolor activator 7 ƒw z 15 ew z w. x 10uL 1mL ƒwš 37 o C 5 incubation k z d w. 11) kw w m w ƒ n z fenofibric acid w k q l(auc inf,, Cl total /F, K a, K el, t 1/2, V d /F) w sƒw. AUC Õ œ w w š d š, d š ùkü w. š j (Cl total /F) n AUC inf ù w. ful v ADAPT II w ƒƒ x l 1 ƒ one compartment open model fittingw compartmental analysis ww. Fitting v l K a, K el w š w» (t 1/2 = 0693/K el ) w. V d /F n AUC inf K el ù w. w y 0 triglyceride» Fig. 1. Molecular structure of fenofibrate (left) and its active metabolite, fenofibric acid (right). Table 2. Pharmacokinetic parameters (mean ± SD) of fenofibric acid in healthy volunteers after a single oral dose of fenofibrate (250 mg; sustained-release capsule) Parameter Fasted condition Standard meal High-fat meal Non-compartmental parameter AUC inf (µg h/mlp 52.32 ± 26.20 128.42 ± 48.07* 174.78 ± 71.87* (µg/ml) 2.39 ± 1.84 6.92 ± 2.67* 9.15 ± 3.46* (hr) 6.38 ± 4.46 7.83 ± 2.46 8.08 ± 4.30* Compartmental parameter V d /F (L) 134.65 ± 92.13 38.30 ± 14.07* 30.21 ± 16.45* K a (L/hr) 1.19 ± 1.58 1.13 ± 1.15 1.19 ± 1.10 K el (L/hr) 0.04 ± 0.01 0.05 ± 0.05 0.05 ± 0.02 T lag (hr) 0.97 ± 0.45 3.36 ± 1.98* 3.83 ± 1.88* AUC inf, area under the curve for plasma concentration vs. time;, peak concentration;, time to reach ; V d /F, volume of distribution; K a, absorption rate constant; K el, elimination rate constant; T lag, lag time of drug absorption. *Significant change from the fasted condition (P < 0.01); Significant change from the standard meal condition (P < 0.05).

r v p e 1z n z kw w sƒ 37 w n z 24 triglyceride y w. l s³ ± t r txw. ANOVA mw sƒw SPSS 11.0 for windows (SPSS inc., Chicago, Illinois, USA) w. x š wr v p e kw z œ k, t w k, š w k r e 3 w kw q l Table 2 ùkü. w ¾ x š w (AUC inf ) œ k, t w k, š w k ƒƒ 52.32, 128.42 174.78 µgáhr/ml. šx ( ) ƒƒ 2.39, 6.92, 9.15 µg/ml d. š x ( ) ƒƒ 6.38, 7.83 8.08 hr. AUC inf œ n w w t w 2.45 ƒw š, š w z n w 3.34 ƒw. ƒƒ 2.89 3.82 ƒw. w w» w two one-sided tests (TOST) mw w 90% 0.80 1.25 ù w q. Schuirmann t-test mw TOST mw w ù kü. Wilcoxon test mw w œ n w w t w, š w w (Table 3). 12) z n w œ n w ƒ non-compartmental q l w (p<0.01). š x (Cmax) š w t w Table 3. Statistical comparisons of pharmacokinetic parameters for fenofibric acid in the fasted, standard meal, and highfat meal conditions 90% C.I. Result of Schuirmann s test Result of Wilcoxon test (0.80 1.25) Side I Side II Std(I):Fast(J) t 1 P t 2 P z P 0.23 0.38 6.98 < 0.01 7.67 < 0.01 AUC t 0.28 0.48 6.66 < 0.01 9.61 < 0.01 3.09 < 0.01 High(I):Fast(J) 0.17 0.29 7.02 < 0.01 9.83 < 0.01 AUC t 0.20 0.34 8.49 < 0.01 11.44 < 0.01 2.60 < 0.01 High(I):Std(J) 0.59 0.98 0.75 0.23 3.56 < 0.01 AUC t 0.57 0.93 0.35 0.36 3.31 < 0.01 0.201 0.84 Statistical analysis was based on a comparison of the results and confidence interval (C.I.) of group J versus I. Std, standard meal condition; Fast, fasted condition; High, high fat meal condition. Table 4. Plasma concentrations of fenofibric acid in the fasted, standard meal, and high-fat meal conditions Time (h) 1 2 3 4 5 6 8 10 12 24 48 72 Fasted Mean 0.21 1.21 1.73 2.15 1.96 1.89 1.82 1.77 1.48 0.97 0.41 0.20 SD 0.23 1.41 1.88 1.67 1.31 1.18 1.05 0.95 0.75 0.4 0.22 0.19 Standard meal Mean 0.01* 0.22 1.16 2.65 4.38* 5.16* 5.59* 5.46* 4.71* 2.36* 0.98* 0.34 SD 0.04 0.47 1.37 2.51 3.15 3.42 3.23 2.05 2.38 1.03 0.54 0.21 High-fat meal Mean 0.05* 1.12 2.16 3.18 5.24* 6.56* 6.85* 6.33* 5.55* 3.53* 1.28* 0.60* SD 0.16 2.57 3.97 4.35 4.13 4.55 3.67 2.86 2.06 1.99 0.81 0.51 *Significant change from the fasted condition (P<0.01); Significant change from the standard meal condition (P < 0.05).

38 Kor. J. Clin. Pharm., Vol. 15, No. 1, 2005 Fig. 2. Plasma concentrations (mean + SD) of fenofibric acid in healthy volunteers (n = 24) after a single oral dose of fenofibrate (sustained-release capsule; 250 mg). The curves are maximum likelihood fits of a one-compartment open model with lag time (see Methods). Fig. 4. Mean percent changes from baseline plasma concentration of triglyceride in each group. *Significant change from baseline plasma concentration of triglyceride (P<0.05). w ùkü (p<0.01). x š w Table 4. œ n w w z n w absorption phase w elimination phase w w (p<0.01). t w z n w š w z n w elimination phase 24-72 w w (p<0.05). ƒ one compartment open model fittingw Fig. 2 ùkü. Compartmental kw q l Table 2 ùkü. (Kel) œ, t, š ƒƒ 0.04, 0.05 0.05 hr -1. s (V d /F) ƒƒ 134.65, 38.30 30.21 L Fig. 3. Plasma concentrations (mean + SD) of triglyceride in healthy volunteers (n = 24) after a single oral dose of fenofibrate (sustained-release capsule; 250 mg) and in control group (n=8). Fig. 5. The percent fenofibric acid absorbed vs. time profiles after an oral administration of fenofibrate. Each data point is the mean value for 24 subjects., (Ka) ƒƒ 1.19, 1.13 1.19 hr -1. (T lag ) ƒƒ 0.97, 3.36 3.83hr. compartmental kw q l s (V d /F) (T lag ) œ n w w w ƒ š yw (p<0.01). wr v p e w z r e w œ, t w z, š w z r e n w w triglyceride d w Fig. 3. w triglyceride y š 4 96.7±56.4mg/dL š ùkþš, t w 2 86.4 ± 53.5mg/dL š ùkü. n triglyceride n z 24 triglyceride y Fig. 4 ùkü. œ n w, š w z n w, t

r v p e 1z n z kw w sƒ 39 w z n w n triglyceride ƒ ƒ 76.7±41.6, 71.8±53.6 75.7±38.4 mg/dl n z 24 56.2±19.2, 62.7±29.3 50.7±17.6 mg/dl ƒƒ 26%, 13%, 33% w w (p<0.05). n w 0 50.2±25.7 mg/dl 24 z 53.7±25.4 mg/dl 7% ƒw w. š Fenofibrate w n ü ƒ w fenofibric acid. w œ fenofibrate 1z n w z fenofibric acid x y x triglyceride y š w. Fenofibric acid AUC inf ƒ œ n w w t w 2, š w 4 ƒw. w x ùkù fenofibrate w e, w y, x ƒ w w w w œ k x z n w x ƒ ƒ š š. 13) Fenofibric acid x ƒ 1-compartmental open model mw š, Wagner-nelson plots mw 1 (Fig. 5). 14) ƒ w œ w z n w w. ƒ ü y w ƒ š š š, w š x ƒ ùkù. w w ü œ ¼ ƒ» š. 12 w k œ n w, š w z n w t w z n w triglyceride 4 ¾ w e ƒw w. n z 4 ¾ triglyceride j n z 4 z w triglyceride ƒ y w. w n w n z 4 z z triglyceride ƒƒ ùkù y w. š n n baseline triglyceride w fenofibraten z 24 triglyceride eƒ w w (p<0.05). w y x w w ùkü. w š w fenofibric acid x g l e w ƒ š, x fenofibric acid e y w ƒ š š. fenofibrate SR capsule 250mg w w j, w e ƒw. x triglyceride w e ƒw w ùkü š, 1z n w x triglyceride ƒ w w. w triglyceride x w» w Ÿ wš» e ƒ v w ƒ. t t û w w w t w,. š x 1. Hans UK, Structure and biochemical effects of fenofibrate. Am J Med. 1987; 83(5): 9-20. 2. Robert WP, The pharmacokinetics and pharmacodynamics of agents proven to raise high-density lipoprotein cholesterol. Am J Cardiol. 2000; 86: 35-40. 3. Jeong SH, Kim MN, Han MY et al. Fenofibrate prevents obesity and hypertriglyceridemia in low-density lipoprotein receptor-null mice. J. metabol. 2003; 53(5): 607-13. 4. Gonzalez FJ, Peters JM, Cattley RC. Mechanism of action of the nongenotoxic peroxisome proliferator-activated receptor-alpha. J Natl Cancer Inst 1998; 90: 1702-9. 5. Kockx M, Gervois PP, Poulain P. Fibrates suppress fibrinogen gene expression in rodents via activation of the peroxisome proliferators-activated receptor-alpha. Blood 1999; 93: 2991-8. 6. Najib J. Fenofibrate in the treatment of dyslipidemia: a review of the data as they relate to the new suprabioavailable tablet formulation. Clin ther. 2002; 24: 2022-50. 7. Balfour JA, Mc Tavish D, Heel RC. Fenofibrate. A

40 Kor. J. Clin. Pharm., Vol. 15, No. 1, 2005 review of its pharmacodynamic and pharmacokinetic properties and therapeutic use in dyslipidemia. Drugs 1990; 40: 260-90. 8. J.Genest, Nguyen NH, Theroux P et al. Effect of micronized fenofibrate on plasma lipoprotein levels and hemostatic parameters of hypertriglyceridemic patients with low levels of high-density lipoprotein cholesterol in the fed and fasted state. J cardiovasc pharmacol 2000; 35(1): 164-72. 9. U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research. Guidance for industry: Food-effect bioavailability and fed bioequivalence studies 2002. p. 1-9. 10. Streel B, Hubert PH, Caccato A. Determination of fenofibric acid in human plasma using automated solidphase extraction coupled to liquid chromatography. J Chromatogr B 2000; 742: 391-400. 11. CH 100 user s manual. SEAC, Italy 12. Guivarc h PH, Micheal G, Diana F. A new fenofibrate formulation: results of six single-dose clinical studies of bioavailability under fed and fasting conditions. Clin Ther 2004; 26: 1456-69. 13. Leonard W, Judith A, Davud T. The influence of food on the absorption and metabolism of drugs. Clin Nutr 1993; 77: 815-29. 14. Leon S, Andrew Y. Applied biopharmaceutics and pharmacokinetics. 4th ed. New York: Prentice-Hall International, Inc. 1999. p. 231-4.