We report the analysis of poppy seed filling for morphine and codeine content. Concentrations in the range 17.4 to 18.6 micrograms/g (morphine) and 2.3 to 2.5 micrograms/g (codeine) were found in different lots of the filling, which is widely used in baking. The effect of consumption of poppy seed filling on opiate urinalysis results is discussed. Morphine concentrations as high as 4.5 mg/L are reported, with persistence of concentrations greater than 0.3 mg/L as long as 35 h after consumption.
The low concentration of hydrocarbons anticipated in pollution baseline studies necessitates the development of analytical techniques sensitive at the sub-microgram per kilogram concentration level. The method of analysis developed in this laboratory involves dynamic headspace sampling for volatile hydrocarbon components of the sample, followed by coupled-column liquid chromatography for the non-volatile components. These techniques require minimal sample handling, reducing the risk of sample component loss and/or sample contamination. Volatile sample components are separated from the matrix in a closed system and concentrated on a TENAX-GC packed pre-column, free from large amounts of solvent and ready for GC/GC-MS analysis. Non-volatile compounds, such as the benzpyrenes, may be extracted from large volumes of water and concentrated on a Bondapak C18 packed pre-column for coupled-column liquid chromatographic separation and analysis. Results of the application of these techniques to the analysis of samples from sites of known low level hydrocarbon contamination are presented and discussed.
The laboratories of the U.S. Customs Service frequently encounter the major analytical problem of determining the country of origin of imported commodities. This is particularly challenging with natural products. This paper will describe the process for one such commodity --pistachio nuts.Two approaches were taken, high performance liquid chromatography (HPLC) and Differential Scanning Calorimetry (DSC). It was found that the results of these two techniques were complimentary and confirmatory. The HPLC data was obtained on the petroleum ether soluble fraction of the pistachio nuts while the DSC runs evaluated both this fraction and the whole nut. The HPLC results were further investigated by collecting fractions from the eluting peaks, derivatizing them to form the methyl ester of the fatty acids, and profiling by gas chromatography to confirm the triglycerides originally present. The U.S. Customs Service is currently using DSC area ratios to screen imported pistachio nuts for country of origin.
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