A Scoping Review on Fungus and Mycotoxin Studies in the Building’s Environment: Mycotoxin Analysis by Mass Spectrometry

Table 4

Mycotoxin analysis using GC-MS-MS/LC-MS-MS.

No.	Analyte/metabolite/mycotoxin	System/instrumentation/method	Validation			Reference
			Precision/accuracy	LOD/LOQ/CV	Recoveries/
1	Fungal aerosols AFB1, B2, G1, G2, M1, diacetoxyscirpenol, gliotoxin, mycophenolic acid, neosolaniol, ochratoxin A, T-2 toxin (method 1); alternariol, deoxynivalenol, deepoxy-deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, fusarenon X, HT-2 toxin, verrucarol, zearalenone (method 2)	HPLC-MS/MS, MRM, positive and negative modes, ESI		Quantification limit (ng/filter): 0.05–0.50	Recovery: 56–101.10%	[21]
2	DON, AFB1, OTA, toxin T-2 (T-2), zearalenone (ZEA), and sterigmatocystin (STE)	HPLC/ESI-MS/MS, MRM, positive and negative modes, ESI, and the ion source temperature of 150°C in splitless mode	The intraday precision: 4% to 8%. The interday precision: 4% to 14%	LOD in the matrix: 0.8 (AFB1) to 8.5 ng·mL^−1 (T-2 toxin) LOQ in the matrix: 3.2 (AFB1) to 26 ng·mL^−1 (T-2 toxin)	Recoveries of all tested mycotoxins (72–95%) with a CV% below 10%. when the matrix-matched standard curve without the ISTD was used	[39]
3	Verrucarol	GC-MS/MS, negative chemical ionization mode using methane as ionization gas at the energy of 150 eV	NIL	NIL	Recovery of verrucarol was 94%	[24]
4	3 mycotoxins (HT-2 toxin, nivalenol, patulin) (method 1); 14 mycotoxins (aflatoxins B1, B2, G1, G2, M1, citrinin, diacetoxyscirpenol, fumagillin, gliotoxin, mycophenolic acid, neosolaniol, ochratoxin A, T-2 toxin, verruculogen) (method 2)	HPLC-MS/MS, MRM, positive and negative modes, ESI	NIL	Quantification limit (ng/filter) ranged from 0.05 to 23.49	Recoveries ranged from 42% (HT-2) to 97% (DAS)	[22]
5	A total of 186 compounds comprise 159 fungal metabolites and 27 bacterial metabolites	Liquid chromatography/tandem mass spectrometry (LC-MS/MS), specifically QTRAP 4000 LC-MS/MS equipped with a TurboIonSpray electrospray ionization source and an 1100 series HPLC system	Positive identification was obtained by the acquisition of two sMRM transitions per analyte that made 4.0 identification points according to decision by 2002/657/EC. The LC RT and the intensity ratio of the two sMRM transitions had to agree with the related values of an external standard within 0.1 min and 30% relative, respectively	Generally, in the low μ/Kg range and exceeded 50 μ/kg only for those compounds exhibiting a low apparent recovery or a general low MS/MS sensitivity	29/36 analytes (81%) tested reached within a target range of 70–120%	[25, 26]; [41]; [42]
6	Aflatoxin B1, gliotoxin, satratoxin G, satratoxin H, and sterigmatocystin; Trichodermol and verrucarol	HPLC-MS. A ProStar HPLC/1200L triple-quadrupole MS-MS system was used, 5 μM C18-A 150 by 2.0 mm RP-18 column equipped with a MetaGuard 2.0-mm 5 μM C18-A precolumn. Reserpine was used as the internal standard; GC-MS-MS using a CP-3800 GC-triple-quadrupole MS-MS system. The derivatives were analyzed by using MS-MS in negative ion chemical ionization mode, at an energy of 70 eV and an ion source temperature of 150°C, and with ammonia as the ionization gas	The electrospray ionization MS parameters achieved maximal detection sensitivity for each standard when their spectrum showed prominent parent and product ions	Trichodermol and verrucarol 6 pg, sterigmatocystin 12 pg, and aflatoxin B1 and gliotoxin 125 pg; Satratoxins G and H were not quantified	The recovery value was 53 ± 6% with 11.2% CV	[28, 42–43]
7	A total of 186 compounds comprise 159 fungal metabolites and 27 bacterial metabolites; Trichodermol & verrucarol	Liquid chromatography/tandem mass spectrometry (LC-MS/MS), specifically QTRAP 4000 LC-MS/MS equipped with a TurboIonSpray electrospray ionization source (ESI) and an 1100 series HPLC system. Elution was carried out in binary gradient mode; GC-triple-quadrupole MS/MS instrument	Positive identification was obtained by the acquisition of two sMRM transitions per analyte that made 4.0 identification points according to decision by 2002/657/EC.; The MSMS conditions were optimized by repeatedly injecting 0.1–1 ng amounts of standards at different collision energy, ion source temperature, and argon pressure in the collision cell. The parameters that gave the largest product ion peak area were selected. Detection sensitivity, defined as amounts of standards injected with a signal-to-noise ratio >4	Generally, in the low μ/kg range and exceeded 50 μ/kg only for those compounds exhibiting a low apparent recovery or a general low MS/MS sensitivity	29/36 analytes (81%) tested reached within a target range of 70–120%	[26, 29, 42, 43]
8	Airborne sterigmatocystin STC	HPLC/UC-VIS	NIL	Quantification limit (0.025–250.0 μg/ml)	values: 0.9999	[30]
9	Sterigmatocystin roquefortine C	HPLC Waters analytical column	NIL	Limit of determination of the method: 0.2 μg/ml; Quantification limit: 0.2–10 μg/ml	NIL	[26]
10	HPLC-MS-MS; Aflatoxin B; Gliotoxin; Satratoxin G; Satratoxin H; Sterigmatocystin; GC-MS-MS; Trichodermol; Verrucarol	HPLC-MSMS (HPLC/1200L triple-quadrupole MS-MS system). The capillary temperature was 310°C, the capillary voltage was 40 V, the needle voltage was 5,000 V, and the electron multiplier voltage was 2,000 V. The MS spectra were collected as centroid data from m/z 100 to 800, with a scan time of 0.5 s and a scan width of 0.7 s; GC-MS-MS (CP-3800): the derivatives were analyzed by using MS-MS in negative ion chemical ionization mode, at an energy of 70 eV and an ion source temperature of 150°C, and with ammonia as the ionization gas (0.4 kPa)	NIL	LOD: 6 pg; Trichodermol and verrucarol; 12 pg sterigmatocystin; 125 pg aflatoxin B and gliotoxins	NIL	[40]
11	Satratoxin G (SG), satratoxin H (SH), verrucarin J (VerJ), roridin L2 (RL2), mycophenolic acid (MPA), and sterigmatocystin (STC)	UPLC coupled to a Xevo triple-quadrupole mass spectrometer. Quantification was carried out by multiple reaction monitoring (MRM) mode in positive electrospray ionization (ESI)	NIL	LOD: (1) MPA, STC = 0.2 ng/mL; (2) RL2 = 0.2 ng/mL; (3) VerJ = 5 ng/mL; (4) SH, SG = 10 ng/mL; LOQ: (1) MPA, STC, RL2, VerJ = 10 ng/mL; (2) SG, SH = 100 ng/mL	NIL	[32]
12	Satratoxin H; Satratoxin G; Roridin L2; Roridin E; Atranone A; Atranone B; Dolabellane; Stachybotrylactam; Stachybotrylactam (isomer); Stachybotryamide; Stachybotrydial; Mer-NF-5003-B; Trichodermin	UHPLC-QTOF to UHPLC-QqQ	NIL	LOD and LOQ (ng/cm^2), respectively: Satratoxin H (15, 50); Satratoxin G (15, 50); Roridin L2 (0.1, 0.2); Roridin E (0.1, 0.2); Atranone A (2, 6); Atranone B (2, 6); Dolabellane (2, 6); Stachybotrylactam (2, 6); Stachybotrylactam isomer (2, 6); Stachybotryamide (2, 6); Stachybotrydial (2, 6); Mer-NF-5003-B (2, 6); Trichodermin (5, 17)		[31]
13	Aflatoxin B1; Sterigmatocystin; Gliotoxin; Ochratoxin	Dionex Ultimate 3000 UPHLC mass spectrometry detection was carried out on a Q Exactive mass spectrometer (Thermo Fisher Scientific™) operated in positive electrospray ionization (ESI (+)) mode	NIL	Mass spectrometry LOQ; 0.1 ng·mL^−1; (i) Aflatoxin B1; (ii) Gliotoxin; (iii) Sterigmatocystin; 0.2 ng·mL^−1; (i) Ochratoxin A		[23]
14	71 volatile organic compounds; 18 microbial volatile organic compounds	Agilent 6890 GC QTRAP 4000 LC-MS/MS with C18 column	NIL	3 μg/kg for; (i) Sterigmatocystin	Less than 50%	Vishwanath et al. 2011 [26]