Determination of the surface free energy of crystalline and amorphous lactose by atomic force microscopy adhesion measurement.
OBJECTIVE
This study was conducted to accurately measure the dispersive surface free energy of lactose solids in ordered and disordered states.


METHODS
Atomic force microscopy (AFM) was used to determine the contact adhesion force between an AFM tip and lactose under low humidity (ca. 1% RH). The geometry of the tip contacting apex was characterized by scanning a porous aluminum film with ultrasharp spikes (radius 2-3 nm). A sphere vs. flat surface model was employed to relate the adhesion force determined to the surface energy based upon the Johnson-Kendal-Roberts theory. Spray-dried amorphous lactose in a compressed-disk form and single crystals of alpha-lactose monohydrate were prepared as model samples.


RESULTS
The condition of the smooth sample surface and sphere-shaped tip used was shown to be appropriate to the application of the JKR model. The surface energy of crystalline [(0,-1,-1) face] and amorphous lactose was determined to be 23.3 +/- 2.3 and 57.4 +/- 7.9 mJ m(-2), respectively.


CONCLUSIONS
We have demonstrated the capability of AFM to measure the dispersive surface free energy of pharmaceutical materials directly through a blank probe at the nanometer scale. These data, although consistent with results from more traditional methods, illustrate some unique attributes of this approach, namely, surface energies are directly derived from solid-solid interactions, measurements may be made on specific crystalline faces, and the potential exists to identify the submicron heterogeneity of organic solids in terms of their molecular energy states (such as ordered and disordered lactose).
Zhang
Jianxin
J
Molecular Profiles Ltd., 8 Orchard Place, Nottingham Business Park, Nottingham, NG8 6PX, UK.
Ebbens
Stephen
S
Chen
Xinyong
X
Jin
Zheng
Z
Luk
Shen
S
Madden
Claire
C
Patel
Nikin
N
Roberts
Clive J
CJ
D000465:Algorithms; D003460:Crystallization; D007785:Lactose / Q000737:chemistry*; D018625:Microscopy, Atomic Force; D011208:Powders; D013499:Surface Properties; D000267:Tissue Adhesions
D011208:Powders; D007785:Lactose