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Following enzymatic hydrolysis of urine, a gas chromatography–mass spectrometry method for the simultaneous determination of codeine, morphine, hydrocodone, and hydromorphone uses hydroxylamine to form oxime derivatives of the keto-opiates (i.e., hydrocodone, hydromorphone, oxycodone, and oxymorphone). These trimethylsilyl-derivatized forms no longer interfere with the detection and quantitation of codeine and morphine. Samples are extracted on solid-phase columns and quantitated by deuterated internal calibrations of each analyte with selected ion monitoring. Codeine, morphine, hydrocodone, and hydromorphone are completely separated, allowing simultaneous quantitation without interference and a chromatographic analysis time <9 min.

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