A method using liquid chromatography tandem mass spectrometry (LC-MS-MS) with electrospray for the analysis of acrylamide in foods is reported. The method comprises the addition of deuterium-labelled acrylamide-d₃, extraction with water, mixed mode solid phase extraction, ultrafiltration and a graphitised carbon column for chromatography. The transitions m/z 72>55, 72>54, 72>44, 72>27, 72>72 and 75>58 were recorded in multiple reaction monitoring mode for identification and quantification. In-house validation data for products from potatoes and cereals (30 to 10 000 μg kg⁻¹) are presented (accuracy 91 to 102%, relative standard deviation 3 to 21%). Interlaboratory validation data (comparison with gas chromatography mass spectrometry, 25 to 2000 μg kg⁻¹) showed excellent results (r² = 0.998).

A highly specific method for the analysis of β-N-methylamino-L-alanine (BMAA) by LC-MS/MS (liquid chromatography tandem mass spectrometry) has been developed and applied for cycad seeds and cyanobacteria. BMAA was analysed as a free fraction or as total BMAA after acidic hydrolysis to release any protein-bound BMAA. Deuterium labelled BMAA was synthesised and used as internal standard. The method comprises HILIC (hydrophilic interaction chromatography) and positive electrospray ionisation of the native compound, i.e. no derivatisation was used. For safe identification five specific product ions (m/z 102, 88, 76, 73 and 44), all derived from a precursor ion of m/z 119 and originating from different parts of the molecule, were detected (typical relative abundance 100%, 16%, 14%, 12% and 22% respectively). Cyanobacteria or muscle tissue was spiked with BMAA (10 to 1000 µg g⁻¹) to validate the method (accuracy 95% to 109%, relative standard deviation 1% to 6%). The detection limit for free and total BMAA in tissue was <1 µg g⁻¹ and <4 µg g⁻¹ respectively. BMAA was successfully identified and quantified in cycad seeds, whereas previously reported findings of BMAA in samples of cyanobacteria could not be confirmed. Instead, the presence of α-,γ-diamino butyric acid (DAB), an isomer of BMAA, was confirmed in one sample. The possible implications of this finding are discussed.

A non-target analysis method for unexpected contaminants in food is described. Many current methods referred to as “non-target” are capable of detecting hundreds or even thousands of contaminants. However, they will typically still miss all other possible contaminants. Instead, a metabolomics approach might be used to obtain “true non-target” analysis. In the present work, such a method was optimized for improved detection capability at low concentrations. The method was evaluated using 19 chemically diverse model compounds spiked into milk samples to mimic unknown contamination. Other milk samples were used as reference samples. All samples were analyzed with UHPLC-TOF-MS (ultra-high-performance liquid chromatography time-of-flight mass spectrometry), using reversed-phase chromatography and electrospray ionization in positive mode. Data evaluation was performed by the software TracMass 2. No target lists of specific compounds were used to search for the contaminants. Instead, the software was used to sort out all features only occurring in the spiked sample data, i.e., the workflow resembled a metabolomics approach. Procedures for chemical identification of peaks were outside the scope of the study. Method, study design, and settings in the software were optimized to minimize manual evaluation and faulty or irrelevant hits and to maximize hit rate of the spiked compounds. A practical detection limit was established at 25 μg/kg. At this concentration, most compounds (17 out of 19) were detected as intact precursor ions, as fragments or as adducts. Only 2 irrelevant hits, probably natural compounds, were obtained. Limitations and possible practical use of the approach are discussed.

A method using liquid chromatography tandem mass spectrometry (LC-MS-MS) with electrospray (ES) for the determination of traces of narasin, monensin and salinomycin in chicken liver and eggs was developed, validated and used for routine surveillance. The essence of this paper is to demonstrate that one single method can serve very well for two entirely different purposes, i.e., screening and confirmation. Highly reliable confirmation of the identity at low concentrations was demonstrated when residues of narasin were detected and quantified (0.2 to 11 ng g⁻¹) in 50% of the Swedish eggs analysed in 1999. Four daughter ions were detected with ion ratios meeting suggested confirmation criteria for the European Union, even at 0.2 ng g⁻¹. The method was found to be highly cost-effective since both screening and confirmation of 98 liver samples were performed in only two analytical runs (the Swedish national surveillance scheme of 1999, report level 5 ng g⁻¹). The high performance of the method for the different applications was possible due to a combination of the power of ES-LC-MS-MS, a procedure involving screening of pooled samples, and method optimisation of the work-up (automated solid phase extraction), LC and MS parameters. Validation data for narasin (0.5 to 20 ng g⁻¹) in eggs are presented (accuracy 94 to 108%, relative standard deviation 4 to 10%, limit of detection 0.026 ng g⁻¹). The time for an LC-MS-MS run was 4 min, corresponding to 48 s per sample in a pool.

A method that uses mass spectrometry (MS) for identification and quantification of protein toxins, staphylococcal enterotoxins A and B (SEA and SEB), in milk and shrimp is described. The analysis was performed using a tryptic peptide, from each of the toxins, as the target analyte together with the corresponding ¹³C-labeled synthetic internal standard peptide. The performance of the method was evaluated by analyzing spiked samples in the quantification range 2.5–30 ng/g (R² = 0.92–0.99). The limit of quantification (LOQ) in milk and the limit of detection (LOD) in shrimp was 2.5 ng/g, for both SEA and SEB toxins. The in-house reproducibility (RSD) was 8%–30% and 5%–41% at different concentrations for milk and shrimp, respectively. The method was compared to the ELISA method, used at the EU-RL (France), for milk samples spiked with SEA at low levels, in the quantification range of 2.5 to 5 ng/g. The comparison showed good coherence for the two methods: 2.9 (MS)/1.8 (ELISA) and 3.6 (MS)/3.8 (ELISA) ng/g. The major advantage of the developed method is that it allows direct confirmation of the molecular identity and quantitative analysis of SEA and SEB at low nanogram levels using a label and antibody free approach. Therefore, this method is an important step in the development of alternatives to the immune-assay tests currently used for staphylococcal enterotoxin analysis.