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A suite of three ginkgo-containing dietary supplement Standard Reference Materials (SRMs) has been issued by the National Institute of Standards and Technology (NIST) with certified values for flavonoid aglycones, ginkgolides, bilobalide, and selected toxic trace elements. The materials represent a range of matrices (i.e., plant, extract, and finished product) that provide different analytical challenges. The constituents have been determined by at least two independent analytical methods with measurements performed by NIST and at least one collaborating laboratory. The methods utilized different extractions, chromatographic separations, modes of detection, and approaches to quantitation. The SRMs are primarily intended for method validation and for use as control materials to support the analysis of dietary supplements and related botanical materials.

A novel method for the forensic analysis of commercial petroleum products is presented. In this approach, the petroleum sample is extracted with nitromethane and then separated by capillary liquid chromatography with laser-induced fluorescence detection. The addition of selective fluorescence quenching agents allows the sample to be profiled by the distribution of alternant and nonalternant polycyclic aromatic hydrocarbons (PAHs). In preliminary studies, the quenching behavior of nitromethane and diisopropylamine was established by using a standard mixture of sixteen PAHs ranging in size from two to six aromatic rings. Subsequent examination of new and used motor oil demonstrated that characteristic differences arise in the PAH content, which may allow for the unique identification of oil from a particular engine or vehicle. In addition, three brands of petrolatum jelly were successfully distinguished. Although a number of alternant alkylated and heterocyclic PAHs were found in all petrolatum samples, there were significant differences in the relative concentrations of alternant as well as nonalternant PAHs. This allowed for clear differentiation of the samples through qualitative inspection of their chromatograms as well as quantitative statistical correlation techniques.

The retention of six polycyclic aromatic hydrocarbons (PAHs) was characterized by reversed-phase liquid chromatography. The PAHs were detected by laser-induced fluorescence at four points along an optically transparent capillary column. The profiles were characterized in space and time using an exponentially modified Gaussian equation. The resulting parameters were used to calculate the retention factors, as well as the concomitant changes in molar enthalpy and molar volume, for each PAH on monomeric (2.7 micromol/m2) and polymeric (5.4 micromol/m2) octadecylsilica. The changes in molar enthalpy become more exothermic as ring number increases and as annelation structure becomes less condensed. The changes in molar volume become more negative as ring number increases for the planar PAHs, but are positive for the nonplanar solutes. In addition, the rate constants, as well as the concomitant activation enthalpy and activation volume, are calculated for the first time. The kinetic data demonstrate that many of the PAHs exhibit very fast transitions between the mobile and stationary phases. The transition state is very high in energy, and the activation enthalpies and volumes become greater as ring number increases and as annelation structure becomes less condensed. The changes in thermodynamic and kinetic behavior are much more pronounced for the polymeric phase than for the monomeric phase.

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