Ultra-fast retroactive processing by MetAlign of liquid chromatography/high-resolution full-scan Orbitrap mass spectrometry data in WADA Human Urine Sample Monitoring Program.

RATIONALE: The World Antidoping Agency (WADA) Monitoring program concentrates analytical data from the WADA Accredited Laboratories for substances which are not prohibited but whose potential misuse must be known. The WADA List of Monitoring substances is updated annually, where substances may be removed, introduced or transferred to the Prohibited List, depending on the prevalence of their use. Retroactive processing of old sample datafiles has the potential to create information for the prevalence of use of candidate substances for the Monitoring List in previous years. MetAlign is a freeware software with functionality to reduce the size of liquid chromatography (LC)/high-resolution (HR) full-scan (FS) mass spectrometry (MS) datafiles and to perform a fast search for the presence of substances in thousands of reduced datafiles. METHODS: Validation was performed to the search procedure of MetAlign applied to Anti-Doping Lab Qatar (ADLQ)-screened LC/HR-FS-MS reduced datafiles originated from antidoping samples for tramadol (TRA), ecdysterone (ECDY) and the ECDY metabolite 14-desoxyecdysterone (DESECDY) of the WADA Monitoring List. Searching parameters were related to combinations of accurate masses and retention times (RTs). RESULTS: MetAlign search validation criteria were based on the creation of correct identifications, false positives (FPs) and false negatives (FNs). The search for TRA in 7410 ADLQ routine LC/HR-FS-MS datafiles from the years 2017 to 2020 revealed no false identification (FPs and FNs) compared with the ADLQ WADA reports. ECDY and DESECDY were detected by MetAlign search in approximately 5% of the same cohort of antidoping samples. CONCLUSIONS: MetAlign is a powerful tool for the fast retroactive processing of old reduced datafiles collected in screening by LC/HR-FS-MS to reveal the prevalence of use of antidoping substances. The current study proposed the validation scheme of the MetAlign search procedure, to be implemented per individual substance in the WADA Monitoring program, for the elimination of FNs and FPs.

Indoor phthalates from household dust in Qatar: implications for non-dietary human exposure.

Phthalates are ubiquitous semi-volatile organic compounds in the indoor environment present in various consumer products such as cosmetics, polyvinylchloride (PVC) flooring, food packing, and many others. Indoor phthalate concentrations were investigated in 15 buildings including 11 homes, 3 laboratories, and 1 from a hospital in Qatar. Dust samples were collected from vacuum cleaning bags usually used for cleaning homes, labs, and hospitals. The main objectives of this study was to determine the occurrence and concentration of phthalates in dust in Qatar and consequently to estimate the non-dietary human exposure. Eleven phthalates was analyzed. The major identified phthalate compounds at homes in Qatar were bis(2-ethylhexyl) phthalate unlabeled (DEHP) and diisononyl phthalate (DINP) at a geometric mean of 288 µg/g (median 395 µg/g) and 106 µg/g (median 101 µg/g) accounting for 57% and 23% of the total measured phthalates, respectively. The major phthalate compounds found in the first lab building were DEHP and DINP with a median of 4861 µg/g and 943 µg/g, respectively, accounting for 82% and 16% of the total phthalates. For the second lab building, the major phthalates were DEHP with a median of 466 µg/g, accounting for 20% of the total phthalates measured, and DINP median of 1725 µg/g, accounting for 71% of the total measured phthalates. The dust sample tested from hospital building had DEHP as the major phthalate compound with a median of 793 µg/g, accounting for 4.0% of the total measured phthalates, and DINP with a median of 19,626 µg/g, accounting for 94%. The estimated human non-dietary exposure for children, adults, and toddlers was based on phthalate concentrations (median) and found to be 225 ng/kg bw/day for children, 2328 ng/kg bw/day for adults, and 2099 ng/kg bw/day for toddlers.

Development of QuEChERS Method for the Determination of Polycyclic Aromatic Hydrocarbons in Smoked Meat Products Using GC-MS from Qatar.

A simple and fast method for the determination of PAHs in smoked meat samples was described. The QuEChERS (Z-Sep) procedure was used for sample preparation. Gas chromatograph-mass spectrometer with electron ionization (EI) was used to separate and detect the PAHs. All 16 common PAHs were analyzed successfully. Matrix-matched calibration was applied. Spiked samples were performed at 1 ng/g (n=10) and 10 ng/g (n=10) for two days. Overall recoveries of PAHs were within 74 to 117%, with RSDs within 1.15 to 37.57% and 1 and 10 ng/g wet weight for first and second day, respectively. In most of the analyzed smoked meat samples, there were no exceeded levels compared to the maximum levels declared by Commission Regulation (EU) number 835/2011. The method can be recommended for routine analysis for laboratories having a large number of samples.