A nondestructive and noninvasive method to determine water content in lyophilized proteins using low-field time-domain NMR.

Determining the moisture content in lyophilized solids is a fundamental step towards predicting the quality and stability of lyophilized products, but conventional methods are time-consuming, invasive, and destructive. High levels of residual moisture in a lyophilized product can lead to cake collapse, product degradation, and reduced shelf life. The aim of this study was to develop a fast, noninvasive, nondestructive, and inexpensive method for determining the moisture content in a lyophilized monoclonal antibody (mAb) formulation using benchtop low-field time-domain nuclear magnetic resonance spectroscopy.

Finding the right fit: studying the biomechanics of under-tapping with varying thread depths and pitches.

BACKGROUND CONTEXT: Compromise of pedicle screw purchase is a concern in maintaining rigid spinal fixation, especially with osteoporosis. Little consistency exists among various tapping techniques. Pedicle screws are often prepared with taps of a smaller diameter, which can further exacerbate inconsistency. PURPOSE: The objective of this study was to determine whether a mismatch between tap thread depth (D) and thread pitch (P) and screw D and P affects fixation when under-tapping in osteoporotic bone. STUDY DESIGN: This study is a polyurethane foam block biomechanical analysis. MATERIALS AND METHODS: A foam block osteoporotic bone model was used to compare pullout strength of pedicle screws with a 5.3 nominal diameter tap of varying D's and P's. Blocks were sorted into seven groups: (1) probe only; (2) 0.5-mm D, 1.5-mm P tap; (3) 0.5-mm D, 2.0-mm P tap; (4) 0.75-mm D, 2.0-mm P tap; (5) 0.75-mm D, 2.5-mm P tap; (6) 0.75-mm D, 3.0-mm P tap; and (7) 1.0-mm D, 2.5-mm P tap. A pedicle screw, 6.5 mm in diameter and 40 mm in length, was inserted to a depth of 40 mm. Axial pullout testing was performed at a rate of 5 mm/min on 10 blocks from each group. RESULTS: No significant difference was noted between groups under axial pullout testing. The mode of failure in the probe-only group was block fracture, occurring in 50% of cases. Among the other six groups, only one screw failed because of block fracture. The other 59 failed because of screw pullout. CONCLUSIONS: In an osteoporotic bone model, changing the D or P of the tap has no statistically significant effect on axial pullout. Osteoporotic bone might render tap features marginal. Our findings indicate that changing the characteristics of the tap D and P does not help with pullout strength in an osteoporotic model. The high rate of fracture in the probe-only group might imply the potential benefit of tapping to prevent catastrophic failure of bone.

Synthesis and Characterization of an Alumina Forming Nanolaminated Boride: MoAlB.

The 'MAlB' phases are nanolaminated, ternary transition metal borides that consist of a transition metal boride sublattice interleaved by monolayers or bilayers of pure aluminum. However, their synthesis and properties remain largely unexplored. Herein, we synthesized dense, predominantly single-phase samples of one such compound, MoAlB, using a reactive hot pressing method. High-resolution scanning transmission electron microscopy confirmed the presence of two Al layers in between a Mo-B sublattice. Unique among the transition metal borides, MoAlB forms a dense, mostly amorphous, alumina scale when heated in air. Like other alumina formers, the oxidation kinetics follow a cubic time-dependence. At room temperature, its resistivity is low (0.36-0.49 µΩm) and - like a metal - drops linearly with decreasing temperatures. It is also a good thermal conductor (35 Wm(-1)K(-1) at 26 °C). In the 25-1300 °C temperature range, its thermal expansion coefficient is 9.5 × 10(-6 )K(-1). Preliminary results suggest the compound is stable to at least 1400 °C in inert atmospheres. Moderately low Vickers hardness values of 10.6 ± 0.3 GPa, compared to other transition metal borides, and ultimate compressive strengths up to 1940 ± 103 MPa were measured at room temperature. These results are encouraging and warrant further study of this compound for potential use at high temperatures.