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Octreotide and the internal standard, triptorelin, were precipitated from the matrix, washed with dichloromethane and subsequently separated by reversed\u2010phase high\u2010performance liquid chromatography (HPLC) employing a 1% formic acid\/methanol gradient system. Detection was by electrospray ionization mass spectrometry in the positive ion mode using multiple\u2010reaction monitoring. The assay was linear in the concentration range 0.0500\u201350.0\u2009ng\/mL with intra\u2010 and inter\u2010day precision (as relative standard deviation) of &lt;2.95% and &lt;8.37%, respectively. The limit of detection was 0.0200\u2009ng\/mL. The method was applied to a pharmacokinetic study of long\u2010acting released octreotide in healthy volunteers given an intramuscular injection containing 20\u2009mg octreotide. 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