Methyl Esterification Combined with Gas Chromatography-Mass Spectrometry (GC-MS) for Determining the Contents of Lubricant to Evaluate the Compatibility of Chlorinated Butyl Rubber Stoppers with Liposome Injections

A simple, sensitive, and exact methyl esterification in combination with gas chromatography-mass spectrometry (GC-MS) method was developed to determine the contents of palmitic acid and stearic acid in the chlorinated butyl rubber stoppers and liposome injections in order to evaluate the compatibility of pharmaceutical packaging materials. In this experiment, palmitic acid and stearic acid were detected in the form of methyl hexadecanoate and methyl stearate in chlorinated butyl rubber stoppers and liposome injections. The results showed good linearities in the range of 0.50–10.00 µg·mL−1 for methyl hexadecanoate and 1.00–20.00 µg·mL−1 for methyl stearate, with the limits of detection (LOD) 11.94 ng·mL−1 and 11.90 ng·mL−1, respectively. The recoveries that ranged from 95.25% to 100.29% were satisfied, and the relative standard deviation (RSD) was no more than 7.16%. The developed method was successfully applied to evaluate the compatibility of chlorinated butyl rubber stoppers with liposome injections and the safety assessment.

Preparation and Properties Analysis of Chlorinated Butyl Rubber (CIIR)/Organic Diatomite Damping Composites

In this work, a novel type of diatomite was prepared with a limited content of hindered phenol groups grafted on its hydrophobic surface. The obtained samples were characterized for their surface groups, particle morphology, pore structure, and thermal behaviors. Then, modified diatomite (MDT) was used in preparation of reinforced chlorinated butyl rubber (CIIR) composites by mechanical blending method. The powder of MDT can be uniformly dispersed in CIIR matrices and the compatibility was good. In addition, the MDT showed a positive effect on damping performance of CIIR composites. A blending ratio of CIIR/MDT = 100/10 presented the best damping performance and the damping temperature range (tan δ > 0.7) was extended from 60 to 70 °C. The variable temperature FTIR spectra showed the presence of hydrogen bonds between the hydroxyl groups and chloride atoms in the CIIR matrices, and a blue shift exhibited when these hydrogen bonds were dissociated. Hence, these CIIR composites provided good damping behaviors and supplied a novel and promising way for preparation of high damping rubber composites with broad temperature ranges.