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Table 3 QuEChERS extraction of pharmaceuticals from soils

From: Validation of a modified QuEChERS method for the extraction of multiple classes of pharmaceuticals from soils

Type of soil and location

Analyte

Extraction procedure

Clean-up procedure

Analytical methods

Recovery

References

Sandy silty clay soil, local field, Hérault, France

Diclofenac

The extraction was in accordance with Montemurro et al. [45] that tested different levels of acidification of the extraction solvent with formic acid (0.5 and 1%) or ammonium acetate

50 mg PSA, 150 mg C18, 900 mg MgSO4. Acidification was also evaluated after the cleaning phase by adding 0.05% formic acid

SCIEX ExionLCâ„¢ AD system coupled with the SCIEX X500R QTOF system (Sciex, Redwood city, CA, U.S.) with Turbo Vâ„¢ source and Electrospray Ionization (ESI) operating in positive and negative mode

1–30 ng g−1

[46]

Carbamazepine

Metoprolol

Clarithromycin

Climbazole

Clay-loam soil not treated with manure or sludge, location not specified

Carbamazepinea

5 g of soil were spiked at 50 ng/g with MeOH solution containing 31 contaminants. 15 mL of ACN were added to the tube and the AOC acetate buffer was used in the extraction phase

Two steps of clean-up: SAX cartridge and Strata-X cartridge after conditioning the cartridges themselves with MeOH and 0.04 M citric acid

HP1100 chromatographic system. The LC system was coupled to a triple-stage quadrupole mass spectrometer 3200 QTrap with an electrospray ion (ESI) source (TurboV, AB Sciex)

> 90%

[28, 38]

Agricultural soils, location not specified

Clarithromycin

1 g of soil was extracted with ACN acidified or not with acetic acid; 6 g of Na2SO4 as separation salt with or without NaOAc

50 mg PSA, 150 mg C18 sorbent and 900 mg of Na2SO4

Ultra-High-Performance-Liquid Chromatography (UHPLC) Acquity system coupled to a 5500 QTRAP hybrid quadrupole-linear ion trap tandem mass spectrometer (QqLIT AB Sciex, Foster City, CA, USA)

90.2–103.1% for clarithromycin n.r.-144.7% for tetracycline according to the different solvents and salts adopted

[44]

Tetracycline

Soils collected in 29 different points homogenously distributed along the Turia River (Central East of Spain)

Diclofenac Gemfibrozil

1 g of soil was extracted with ACN, and 6 g MgSO4, 1.5 g NaCl, 1.5 g C6H5Na3O7 * 2 H2O, and 0.75 g [HOC(COOH) (CH2COONa)2 1.5 H2O] were added as salts

50 mg PSA, 150 mg anhydrous MgSO4, and 50 mg of C18

1260 Infinity Ultra High-Performance Liquid Chromatograph (UHPLC) system coupled to a 6410 Triple Quad Mass Spectrometry from Agilent Technologies (Santa Clara, CA, USA) to perform tandem mass spectrometry (MS/MS) and an electrospray ionization source in both ion modes

Between 31 and 88%

[47]

Carbamazepine

Clarithromycin Metoprolol

Tetracycline

Diclofenac Gemfibrozil

Agricultural soils (tomatoes), Almeria (Spain)

Carbamazepinea

10 g of soil were extracted with acidified ACN (0.5% v/v, formic acid). 4 g of anhydrous MgSO4, 1 g of Na3Citrate·2H2O, 1 g of NaCl and 0.5 g of Na2HCitrate·1,5H2O were added as salts

750 mg of anhydrous MgSO4, and 125 mg of C18

A Sciex Exion HPLC coupled to a Sciex 6500 + Triple Quad-LC–MS/MS from Sciex

79–88% for carbamazepine, 76–79% for gemfibrozil, 86–99% for diclofenac, according to the different concentrations

[29, 30]

Gemfibrozila

Diclofenaca

Agriculture field (0–20 cm) in Tianjin, China

Clarithromycina

5 g of soils were extracted with Na2EDTA, ACN, and phosphate, acetate or citrate buffer, and NaCl as salt

d-SPE adsorbents (25 mg of PSA,10 mg of C18, and 100 mg of MgSO4)

UHPLC–MS/MS consisted of a Waters Acquity UPLCTM (Waters, USA) equipped with an ACQUITY UPLC BEHTMC18column (1.8 μm; 2.1 mm × 100 mm)

103.9–113.8%, according to the different buffers

[49]

  1. aAuthors validated the method