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* Blood LC-MS/MS screening for 69 NPS and amphetamines was developed and validated.

* Extraction procedure is simple and fast through deproteinization with acetonitrile.

* High identification efficiency and sensitivity were allowed by dynamic MRM mode.

* LLOQ was 0.1 ng/mL for synthetic cannabinoids and 0.3 ng/mL for cathinones.

* The procedure was successfully applied to three real cases.

(C) 2016Elsevier, Inc.