Analysis of unknown (unlabeled/mislabeled) drug products for active pharmaceutical ingredients and related substances by an international mail facility satellite laboratory equipped with rapid screening devices.

Two chemists employed a three-device rapid screening "toolkit" consisting of a handheld Raman spectrometer, transportable mass spectrometer, and portable Fourier transform infrared (FT-IR) spectrometer at an international mail facility (IMF) satellite laboratory to examine unknown (unlabeled/mislabeled) products for the presence of active pharmaceutical ingredients (APIs). Phase I of this project previously demonstrated that this toolkit was the most effective collection of instruments for identifying APIs in product types collected at IMFs during a nationwide mail blitz and Phase II of this project previously demonstrated that results generated using the toolkit during a satellite laboratory pilot program were as reliable as those generated by a full-service library when two or more of these instruments identify an API. This study (Phase III) described the results of the satellite laboratory toolkit during production mode and encompassed the period ranging from June 2021 through December 2022. During this study, a total of 858 products were examined on-site at the IMF. The satellite laboratory yielded conclusive results for 726 (84.6%) products, which were used to support regulatory action, and identified 132 (15.4%) products that required additional full-service laboratory analyses due to inconclusive results. The satellite and full-service laboratory verified/confirmed at least one API/related substance in 617 (71.9%) products. A total of 709 APIs/related substances were found in the 617 products, and 202 of these 709 compounds were unique/different. Overall, during Phases I through III of this program, 350 different substances have been identified in products collected at IMFs.

Detection of fatty acid ethyl esters in skin surface lipids as biomarkers of ethanol consumption in alcoholics, social drinkers, light drinkers, and teetotalers using a methodology based on microwave-assisted extraction followed by solid-phase microextraction and gas chromatography-mass spectrometry.

Fatty acid ethyl esters (FAEE) are known to be a direct alcohol marker and are mainly investigated in hair samples for their ability to be incorporated into this matrix from sebum. The present study used an already developed methodology to provide and confirm information about the use of FAEEs in skin surface lipids as markers of alcohol consumption. The skin surface lipids were collected with Sebutapes(®) from the foreheads of teetotalers, light drinkers, social drinkers, and alcoholics. The samples were analyzed by direct solid-phase microextraction and gas chromatography-mass spectrometry for ethyl myristate, ethyl palmitate, ethyl oleate, and ethyl stearate. Relative FAEE/sebum allowed an evaluation of alcohol consumption. The ranges obtained for relative FAEEs in each category were as follows, teetotalers (0-13.85 pg/mg), light drinkers (11.10-26.80 pg/mg), social drinkers (20.55-86.55 pg/mg), and alcoholics (109.00-1243.40 pg/mg). A social drinker volunteer was monitored during a period of two months. The highest m(FAEE)/m(sebum) were generally detected 7-9 days after the days of high alcohol consumption. From these results, a clear distinction of teetotalers, social drinkers, and alcoholics could be established with the methodology used.