Optimization of the bake-on siliconization of cartridges. Part II: Investigations into burn-in time and temperature.

Combination products have become popular formats for the delivery of parenteral medications. Bake-on siliconization of glass syringes or cartridges allows good piston break-loose and gliding during injection at low silicone levels. Although widely implemented in industry, still little is known and published on the effect of the bake-on process on the silicone level, layer thickness and chemical composition. In this study, cartridges were bake-on siliconized in a heat-tunnel by varying both temperature from 200 to 350°C for 12min and time from 5min to 3h at 316°C. Furthermore, a heat-oven with air-exchange was established as an experimental model. Heat treatment led to a time- and temperature-dependent decrease in the silicone level and layer thickness. After 1h at 316°C lubrication was insufficient. The silicone levels substantially decreased between 250 and 316°C after 12min. After bake-on, the peak molecular weight of the silicone remained unchanged while fractions below 5000g/mol were removed at 316 and 350°C. Cyclic low molecular weight siloxanes below 500g/mol were volatilized under all conditions. Despite most of the baked-on silicone was solvent-extractable, contact angle analysis indicated a strong binding of a remaining, thin silicone film to the glass surface.

Determination of caffeine, myosmine, and nicotine in chocolate by headspace solid-phase microextraction coupled with gas chromatography-tandem mass spectrometry.

The occurrence of the bioactive components caffeine (xanthine alkaloid), myosmine and nicotine (pyridine alkaloids) in different edibles and plants is well known, but the content of myosmine and nicotine is still ambiguous in milk/dark chocolate. Therefore, a sensitive method for determination of these components was established, a simple separation of the dissolved analytes from the matrix, followed by headspace solid-phase microextraction coupled with gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS/MS). This is the first approach for simultaneous determination of caffeine, myosmine, and nicotine with a convenient SPME technique. Calibration curves were linear for the xanthine alkaloid (250 to 3000 mg/kg) and the pyridine alkaloids (0.000125 to 0.003000 mg/kg). Residuals of the calibration curves were lower than 15%, hence the limits of detection were set as the lowest points of the calibration curves. The limits of detection calculated from linearity data were for caffeine 216 mg/kg, for myosmine 0.000110 mg/kg, and for nicotine 0.000120 mg/kg. Thirty samples of 5 chocolate brands with varying cocoa contents (30% to 99%) were analyzed in triplicate. Caffeine and nicotine were detected in all samples of chocolate, whereas myosmine was not present in any sample. The caffeine content ranged from 420 to 2780 mg/kg (relative standard deviation 0.1 to 11.5%) and nicotine from 0.000230 to 0.001590 mg/kg (RSD 2.0 to 22.1%).