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Journal Article


Rule G, McLaughlin LG, Henion J. Anal. Chem. 1993; 65(19): 857A-863A.


Diagnostic Laboratory, College of Veterinary Medicine, Cornell University, Ithaca, NY 14851-0786.


(Copyright © 1993, American Chemical Society)






This forensic case taught us several lessons. First, there is a need for improved sample cleanup and treatment of severely decayed tissue samples when trace determinations of target analytes are needed. With the exception of a few reports the literature is lacking in information with regard to the most modern sample preparation techniques. Second, the coupling of LC/LC with tandem MS provides an effective means of "on-line" samples cleanup for complex sample matrices. The improvements in selectivity shown in Figure 3 reveal the analytical power available when these techniques are combined. Third, once we decided to use LC/LC/MS/MS, we were able to analyze more than 50 samples in a semi-automated fashion over approximately three days. The reliability and ruggedness of the combined techniques and equipment suggest this approach may have merit for common applications in which large numbers of biological samples (e.g., plasma and urine) must be analyzed. As a postscript, when this project was completed we proposed that the use of antibodies for isolating oleandrin and its relatives might be a more selective means for trace enrichment of the target analytes. For example, a high-pressure immunoaffinity column could have been coupled on line as column 1 in Figure 4. After pumping a relatively high volume of aqueous tissue extract through an immunoaffinity column during trapping and trace enrichment conditions, the column could be rinsed with phosphate-buffered saline. Then the pH could be lowered to unfold the antibody protein and allow release of the trapped analyte from this column with subsequent trapping on column 2 in Figure 4.(ABSTRACT TRUNCATED AT 250 WORDS)

Language: en


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