Analytical Methods for Environmental Contaminants of Emerging Concern. Группа авторов

such as chlorothalonil and TPs (sulphonic acids and phenols) by LC-Orbitrap-MS [90]. However, sometimes these extraction procedures are avoided, and direct injection of water samples, after filtration, can be considered when using LC. In fact, its combination with tandem MS (MS/MS) has allowed for the determination of pesticides at ultra-trace levels in surface and groundwaters [25, 27, 91].

Table 1.1 Overview of analytical methods applied to monitor pesticides in environmental waters.^a

Pesticides	Matrix	Extraction technique	Determination technique	Recovery (%)	LOQ (µg l−1)	Reference
4 OCP and 2 OPPs	Surface water	LLE (dichloromethane)	GC-FID	80–90	0.002	[68]
296 pesticides + 156 pharmaceuticals, 18 consumer products, 10 industrial chemicals and 4 others	Coastal waters	SPE (Oasis HLB and SpePak cartridges)	LC-QTOF-MS	70–130	0.00002–0.300b	[70]
14 pesticides and TPs	Surface waterand drinking water	SPE (Oasis HLB cartridge)	UHPLC-QTrap-MS/MS	85–105	0.01–0.1	[71]
19 acidic herbicides + metabolites	River water	SPE (Oasis HLB cartridge)	LC-QqQ-MS/MS	64–111	0.004–0.022	[72]
6 neonicotinoids and metabolites	Drinking water	SPE (Oasis HLB cartridge)	LC-DAD-QqQ-MS/MS& QTOF-MS	57–120	0.000057–0.000488b	[18]
ca. 500 pesticides and TPs	Surface water and groundwater	SPE (Oasis HLB cartridge)	UHPLC-QTOF-MS	—	—	[23]
8 pesticides + TPs	Surface water	Mix mode SPE:(HLB: WAX: WCX, 2 : 1: 1)	LC-QqQ-MS/MS	43–141	0.00002–0.0056b	[73]
125 pesticides and metabolites + 130 pharmaceuticals and metabolites + 42 antibiotics and metabolites + 63 others	Surface and marine water	SPE (Strata-X and the mixture Strata-X-AW: Strata-X-CW: Isolute ENV + (1 : 1 : 1.5))	LC-LTQ-Orbitrap-MS	83–93	—	[74]
251 contaminants (pesticides, pharmaceuticals or industrial chemicals and their transformation products)	Surface water	Onsite integrative large-volume SPE (HR-X sorbent)	UHPLC-LTQ-Orbitrap MS	60–123	—	[75]
96 including pesticides and TPs	Surface water,groundwater and drinking water	On-line SPE	UHPLC-QqQ-MS/MS	—	0.005–0.025	[24]
51 pesticides	Surface water and groundwater	On-line SPE (Prospekt-2-system)	LC-QqQ-MS/MS	80–125	0.010	[78]
8 pesticides	Surface water and groundwater	QuEChERS (Acetonitrile, MgSO4 and NaCl)	GC-Q-MS	85–103	0.95–13.69	[80]
Cyflumetofen + 2 metabolites	Surface water	QuEChERS (Acetonitrile, MgSO4 and NaCl)	UHPLC-QqQ-MS/MS	79–118	0.7–9.8	[21]
102 pesticides	Surface water and groundwater	SBSE (PDMS) (GC)On-line SPE (LC)	GC-Q-MS (27)UHPLC-QqQ-MS/MS (75)	—	0.015–0.025 (GC)0.005–0.025 (LC)	[77]
10 pesticides	Surface water	HF-LPME	GC-Q-MS	85–115	0.14–1.69	[82]
14 pesticides + 16 PAHs + 26 PCBs + 6 BDEs	Surface water	On-Line SPME (DI, PA fiber)	GC-DFS-HRMS	87–116	0.0001–0.050	[84]
16 pesticides	Surface water, marine water and groundwater	Magnetic SPME with a magnetic DES-based polymeric hydrogel	GC-µECD	61–120	0.006–0.399	[86]
24 pesticides	Surface water	SPME (Novel carbon nanomaterial sorbent)	GC-Q-MS	70–123	0.0007–3.7320	[87]
18 chiral pesticides	Surface water and influent and effluent wastewater	Magnetic SPME (Amino modified multiwalled carbon nanotubes)	LC-QqQ-MS/MS	83–105	0.00035–0.00204	[88]
Pesticides	Matrix	Extraction technique	Determination technique	Recovery (%)	LOQ (µg l−1)	Reference
Chlorothalonil + 6 TPs	Surface water and groundwater	Vacuum-assisted evaporative concentration	LC-Orbitrap-MS	85–110	0.0002–0.010	[90]
215 pesticides and TPs (Method SH2437)30 pesticides(Method LC9045)3 herbicides (glyphosate, AMPA and glufosinate)(Method GLYPH)	Groundwater	SH2437 &: LC9045: Direct injectionGLYPH: derivatization with FMOC prior to on-line SPE	LC-QqQ-MS/MS	78–114	0.001–1.350b0.001–0.028b0.020b	[25]
150 pesticide metabolites	Surface waterand groundwater	Direct injection	LC-QqQ-MS/MS	—	0.003–2.000	[27]
16 polar pesticides + pharmaceuticals	Groundwater	Extraction from passive sampler (POCIS): acetone:methanol	UHPLC-QqQ-MS/MS	42–116	0.00003–0.00135b	[59]

^aAbbreviations: BDEs: Brominated diphenyl ethers; DAD: Diode array detector; DES: Deep eutectic solvent; DFS-HRMS: Magnetic sector high resolution mass spectrometry: DI: Direct injection; FID: Flame ionization detection; FMOC: 9-florenylmethyl-chloroformate; GC: Gas chromatography; HF-LPME: Hollow fiber-liquid phase microextraction; HLB: Hydrophilic-lipophilic balanced; LC: Liquid chromatography; LLE: Liquid-liquid extraction; LOQ: Limit of quantification; LTQ: Linear ion trap; MS: Mass spectrometry; MS/MS: Tandem mass spectrometry; µECD: Micro electron capture detector; OCPs: Organochlorine pesticides; OPPs: Organophosphorus pesticides; PA: Polyacrilate; PAHs: Polycyclic aromatic hydrocarbons; PCBs: Polychlorinated biphenyls; PDMS: Polydimethylsiloxane; POCIS: Polar organic chemical integrative samples; Q: Single quadrupole; QqQ: Triple quadrupole; QTOF: Quadrupole time of flight; QTRAP: Hybrid triple quadrupole-linear ion trap; SBSE: Stir bar sorptive extraction; SPE: Solid phase extraction; SPME: Solid phase microextraction; TPs: Transformation products; UHPLC: Ultra-high-performance liquid chromatography; WAX: Weak anion exchange; WCX: Weak cation exchange.

      ^bLimit of detection.

In relation to solid samples, such as soils, the most common methods were based on solid-liquid extraction (SLE), pressurized liquid extraction (PLE) and QuEChERS (see Table 1.2). In SLE methods, solvent mixtures such as acetonitrile and water have been widely used. For example, a mixture of water/acetonitrile (10 : 90, v/v) was utilized to monitor pesticide residues in soils from Argentina [62], or a mixture of water/acetonitrile (40 : 60, v/v) was used for the extraction of oxanilic and sulfonic acids metabolites [92]. Hu et al. employed methanol:water (50 : 50, v/v) instead of acetonitrile for the extraction of acetochlor and propisochlor in soils from Beijing (China) [63]. Colazzo et al. tested different solvents and mixtures, such as acetonitrile, methanol, water and methanol/water, choosing methanol as the best option (recoveries ranged from 45 to 90%) to determine pesticide residues in paddy fields and sugar cane from Uruguay [93].

Table 1.2 Overview of analytical methods applied to determine pesticides in soil matrices.^a

Pesticides	Extraction	Determination technique	Recovery (%)	LOQ (µg kg−1)	Reference
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