F ~

ELSEVIER

European Journal of Pharmaceutics and Biopharmaceutics 44 (1997) 323-326

Technical note

A new practical index to predict capping occurring during the tableting process
Ken-ichi Sugimori

a,* Yoshiaki Kawashima b

a Central Pharmaceutical Research Institute, Japan Tobacco Inc., Osaka, Japan b Gifu Pharmaceutical University, Gifu, Japan

Received 5 July 1996; accepted 18 August 1997

Keywords: Tablet; Capping; Capping index

1. Introduction

When pharmaceutical powders are compacted into tablets, cracking, usually termed capping, sometimes occurs inside the tablets. Many studies have been done from practical and theoretical viewpoints to overcome this problem [1-3]. The mechanism of capping is, however, not fully understood. Although some indices were proposed to estimate capping tendency [4-6], it is difficult to estimate capping quantitatively with any type of pharmaceutical powders by means of those indices. The present authors described capping as a cracking produced inside the tablet and was induced by residual die wall pressure applied at the final stage of the decompression process [7]. The capping ratio (tendency of capping) of a tablet was represented by (Fu-F)/F,, where F is the crushing strength of a tablet prepared by the normal method and F, is that of an ideally compacted tablet without capping using a loaded-ejectiontype compaction apparatus [7]. The value of the capping ratio varies from zero (without capping) to unity (completely capped). The authors have proposed a capping index (C1) defined by Qr/Pc, where Qr is the residual die wall pressure which is evaluated by extrapolating a linear relationship between the die wall pres* Corresponding author. Central Pharmaceutical Research Institute, Japan Tobacco Inc., 1-1 Murasaki-cho, Takatsuki, Osaka 569, Japan. 0939-6411/97/$17.00 1997 Elsevier Science B.V. All rights reserved. P11 S0939-6411(97)001 31-8

sure and the axial pressure at the final stage of decompression process to zero of axial pressure and P~ is the axial crushing strength of a cylindrical compact. A good correlation was found between the two parameters. Capping always occurred when the capping index exceeded unity and where the residual die wall pressure exceeded the crushing strength. When the capping index was approximately unity, the tablets were partially capped. It was possible to predict capping occurring during tableting by this index. Thus the capping index is very useful for predicting capping during tableting. However, it is difficult to measure the residual die wall pressure unless a special die with a strain gauge is used [8]. In this study, the physical meaning of the capping index was rediscussed more quantitatively and a new useful practical method to find this index was investigated by estimating the residual die wall pressure (Qr) from a crushing test of a cylindrical compact.

2. Materials and methods

2. I. Materials [7]
Caffeine (Shizuoka, Japan), cornstarch (Japan Cornstarch, Japan) and a mixture (2:1) of lactose (DMV, Holland) and cornstarch were used as reference powders without capping tendency. Ethoxybenzamide (ethenzamide, Yoshitomi, Japan), lactose, hydroxy-

324

K.-i. Sugimori, Y. Kawashirna/ European Journal of Pharmaceutics and Biopharmaceutics 44 (1997) 323-326

buthylphenetidin (bucetin, Yamato, Japan) and the granule prepared from ethenzamide (45%), bucetin (45%) and a-starch (10%, Nichiden, Japan) by wet massing were used as powders with capping tendency.

LE 600
400

j,

'

2.2. Tablet preparation [7]

I/I

Tablets were prepared by using a die with 8.5 mm internal diameter, punches with either fiat face or concave face (6.5 mm radius of curvature) and a compacting test apparatus (Autograph, Shimadzu Seisakusho, Japan). The die was lubricated by puffing a very small amount of powdered magnesium stearate (Sakai, Japan) prior to every compaction.

b~

I,.. 4.e

~200

10

Strain (%)
Fig. 2. Stress-strain curves on crushing cylindrical compacts (1 kgf/cm 2 =98.07 kPa) [1]. O, caffeine; A, lactose and cornstarch mixture; [], cornstarch; ~ , ethenzamide and bucetin granule; O, ethenzamide; A, lactose; II, bucetin.

2.3. Measurement of residual die wall pressure [8] and crushing strength [7]
Die wall pressure was measured using a specially designed die with a strain gauge attached to the outer surface of the die. The crushing strength of the compacted powder was measured by compressing axially a flat-faced cylindrical compact (1000 mg weight, 11.3 mm diameter, 7-8.5 mm thickness).

3. Results and discussion

3.1. Physical meaning of the capping index (Cl = Or~Pc)

Fig. 1 (upper) shows the stresses applied on a tablet in a die at the final stage of the decompression process and its Mohr's circle. The tablet is compressed by low axial pressure (P) and high radial pressure (Q). Shear stresses (~) and compressive stress (s) in the tablet are expressed by a Mohr's circle which passes through (P,0)
p 7
t, t

and (Q,0), and shear stress (r) reaches the maximum ( ( Q - P)/2) acting in a direction of 45 degrees. If the shear stress (~) overcomes the shear strength of the compacted powders (%), the tablet may crack in the direction shown in the figure. The Mohr's circle of the tablet at the extrapolated end stage of decompression process is represented by the dotted line, passing through (0,0) and (Or,0), where Or is the residual die wall pressure and Or~2 is the maximum shear stress. The shear strength (%) of compacted powder was estimated from the axial crushing strength of (Pc) a cylindrical compact. Mohr's circle of the compact when crushed is shown in Fig. 2 (lower), which passes through (0,0) and (Pc,0). The shear stress in the compact becomes maximum at a direction of 45 degrees and the compact is cracked in this direction. Therefore the capping index (Or~Pc) is described in terms of the ratio of diameter of solid lined Mohr's circle to dotted line, that is the ratio of maximum shear stress (Or/2) and shear strength of compacted powder (P J2).

"~

TC

3.2. Estimation of residual die wall pressure

O"

' , P

II

Pc
TC

Pc

Fig. 1. Stress and Mohr's circle for a tablet (upper) and for a cylindrical compact (lower).

The results of the crushing test and the residual die wall pressure measurement on a corresponding flatfaced tablet, which were reported in a previous publication [7] are represented in Fig. 2 and Table 1. The powders with lower residual die wall pressure are assumed to indicate higher strain on the axial crushing test of a cylindrical compact. The maximum strain in the crushing test (Smax) was compared to the residual die wall pressure of a flat-faced tablet (Qrf). The relationship between the residual die wall pressure and the reciprocal of maximum strain is shown in Fig. 3. The residual die wall pressure was approximately proportional to the reciprocal of the maximum strain. This means that the residual die wall pressure depends on

K.-i. Sugimori, Y. Kawashima/ European Journal of Pharmaceutics and Biopharmaceutics 44 (1997) 323-326
Table 1 Crushing strength of a cylindrical compact and residual die wall pressure of a flat-faced tablet [7] Material Caffeine Lactose and cornstarch mixture Cornstarch Ethenzamide and bucetine granule Ethenzamide Lactose Bucetine "The unit 1 kgf/cm2 = 98.07 kPa plastic and elastic properties of the powder. Plasticity increases while elasticity decreases residual die wall pressure. The following empirical relationship was obtained between the two parameters. Crushing strength (kgf/cm2) a 505 365 350 390 450 175 165 Maximum strain (%) 3.11 2.68 8.68 1.32 1.16 0.97 1.19 Residualpressure (kgf/cm2) 95 90 5 220 240 195 165

325

Qr, = 236/Smax

(r = 0.91)

(1)

of the flat-faced tablet having the same volume as a convex-faced tablet and Te is the edge thickness of a convex-faced tablet as illustrated in Fig. 4. The shape correction factor (F,) of residual die wall pressure was defined by Eq. (3).

Eq. (1) means that it is possible to estimate the residual die wall pressure on the cylindrical compact using the crushing test. This is a very practical method to estimate the residual pressure.

Fs = Qrc/Qrf = 0.3 q- 0.7Tv/Te

(3)

The residual die wall pressure of a convex-faced tablet can be estimated with the value of a fiat-faced tablet by using Eq. (4).

3.3. Shape correction factor of residual die wall pressure

Usually capping takes place more frequently in convex-faced tablets than fiat-faced tablets, convex-faced tablets showed higher residual die wall pressure than flat-faced [7,8]. A thinner tablet showed higher residual die wall pressure and higher capping ratio. The authors described the following relationship between residual die wall pressure and tablet shape [7].

3.4. Estimation of capping index

It is possible to calculate the capping index (CI) of various shaped tablets without measuring die wall pressure by combining Eqs. (1) and (2) as follows. Clcalc = (235/PcSmax)(0.3 q- 0.7Tv/Tc) (r = 0.94) (4)

(O~c - Orf)/Orf = 0-7(Tv - Te)/Te

(r = 0.97)

(2)

where Qrc and Q r f a r e the residual die wall pressures of convex-faced and fiat-faced tablets, Tv is the thickness
400
!

300

The capping indices of various shaped tablets were calculated using the crushing test results of a cylindrical compact (Pc and Smax) and tablet shape (Tv and Te). The calculated indices were compared with the observed indices which were evaluated using directly measured residual die wall pressure (Fig. 5). A good correlation was obtained between the two indices. This means that it is possible to predict the capping tendency of tablet from the strength and the strain data of a cylindrical compact crushing test. This is a very convenient method to predict compressing behavior of powders and very useful for the practical study of tablet formulation.

~ -g2 0 0

'1=
0

100

I Te
0.5
l/Sm,~

Fig. 3. Relationship between residual die wall pressure and maximum strain (1 kgf/cm2= 98.07 kPa).

Fig. 4. Tv and Te of a tablet (Tv is the thickness of the flat-faced tablet having the same volume of a convex-faced tablet)

326
4.0

K.-i. Sugimori, Y. Kawashima / European Journal of Pharmaceutics and Biopharmaceutics 44 (1997) 323-326 Tv/Te. T h u s tablets w i t h o u t c a p p i n g can be successfully f o r m u l a t e d o r designed using Eq. (4).

3.0

~oO,~~'t~'' o,,~
2.0 1.0

References
[l] P.J. Rue, P.M.R. Barkworth, P. Ridgway-Watt, P. Rough, D.C. Sharland, H. Seager, H. Fisher, Analysis of tablet fracture during tableting by acoustic emission techniques, Int. J. Pharm. Tech. Prod. Mfr. 1 (1979) 2-5. [2] G.E. Amidon, D.P. Smith, E.N. Hiestand, Rotary press utilizing a flexible die wall, J. Pharm. Sci. 70 (1981) 613-617. [3] L. Casahoursat, G. Lemagnen, D. Larrouture, The use of stress relaxation trials to characterize tablet capping, Drug Dev. Ind. Pharm. 14 (1988) 2179-2199. [4] P.J. Jarosz, E.L. Parrot, Factors influencing axial and radial tensile strengths of tablets, J. Pharm. Sci. 71 (1982) 607-614. [5] A.B. Bangudu, N. Pilpel, Effects of composition, moisture and stearic acid on the plasto elasticity and tableting of paracetamol-microcrystalline cellulose mixtures, J. Pharm. Pharmacol. 37 (1985) 289 293. [6] W.E. Jetzer, Measurement of hardness and strength of tablets and their relation to compaction performance of powders, J. Pharm. Pharmacol. 38 (1986) 254 258. [7] K. Sugimori, S. Mori, Y. Kawashima, Introduction of a new index for the prediction of capping tendency of tablets, Chem. Pharm. Bull. 37 (1989) 458-462. [8] K. Sugimori, S. Mori, Y. Kawashima, Characterization of die wall pressure to predict capping of fiat- or convex-faced drug tablets of various sizes, Powder Technol. 58 (1989) 259-264. [9] K. Sugimori, S. Mori, Y. Kawashima, The role of binders in the prevention of capping within a tablet, Chem. Pharm. Bull. 37 (1989) 1064-1067. [10] K. Sugimori, S. Mori, Y. Kawashima, Application of a newly defined capping index in evaluation of the compressibility of pharmaceutical powders, Adv. Powder Technol. 1 (1990) 25 37.

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,
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CI e ~ Fig. 5. Relationship between calculated capping index and observed capping index. O, fiat-faced tablet; o, convex-faced tablet 3.5. Prevention o f capping Eq. (4) suggesfs a w a y t o p r e v e n t c a p p i n g . I n c r e a s i n g Pc decreases c a p p i n g index, l e a d i n g to r e d u c e d c a p p i n g . T h e a d d i t i o n o f b i n d e r with fine p a r t i c l e size o r in a state o f s o l u t i o n effectively increases Pc [9]. I n c r e a s i n g Smax is also effective in r e d u c i n g c a p p i n g . T h e p o w d e r s o f p o l y m e r m a t e r i a l s , such as starch o r cellulose, s h o w higher Smax. T h e a d d i t i o n o f these p o w d e r s is effective in p r e v e n t i o n o f c a p p i n g [10]. T h e s h a p e o f a t a b l e t is a n o t h e r i m p o r t a n t f a c t o r in p r e v e n t i n g c a p p i n g . C o n sidering c o n v e x - f a c e d tablets, tablets w i t h o u t c a p p i n g m a y be o b t a i n e d if p u n c h e s with larger radii o f curvature are e m p l o y e d b e c a u s e this decreases the value o f