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METHOD Unearthing rare treasures

The characterization of a crude mixture of natural products can be difficult, particularly when the sample is small and composed of a complex brew of low-concentration compounds such as steroids. But researchers continue to find ways to extract more information from ever-smaller samples. Frank C. Schroeder of Cornell University and colleagues now offer a powerful demonstration of the sensitivity that can be achieved by capillary NMR spectroscopy of biological samples (J. Am. Chem. Soc. 2005, 127, 10810). The researchers collected and combined whole-body extracts from just 50 members of a rare firefly species. They partially fractionated the mixture and analyzed each fraction by capillary NMR. The resulting spectra led to the identification of 13 new steroids, including the one shown here. Most of the steroids "could not have been characterized in a reasonable amount of time" without capillary NMR, according to Schroeder. "Crude or semipurified natural products extracts" can be characterized "without exhaustive purification," he adds. The approach should "greatly extend the range of accessible natural products research."

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