Solid-phase micro-extraction procedure for the determination of 1,3-dichloro-2-propanol in water by on-fibre derivatisation with bis(trimethylsilyl)trifluoroacetamide.

Solid-phase micro-extraction procedure for the determination of 1,3-dichloro-2-propanol in water by on-fibre derivatisation with bis(trimethylsilyl)trifluoroacetamide.

Analytical and bioanalytical chemistry (2009-04-11)

Antonia María Carro, Paula González, Noelia Fajar, Rosa Antonia Lorenzo, Rafael Cela

PMID19360402

ABSTRACT

The headspace solid-phase micro-extraction technique with on-fibre derivatisation followed by gas chromatography-tandem mass spectrometry has been evaluated for the analysis of 1,3-dichloro-2-propanol in water. An asymmetric factorial design has been performed to study the influence of five experimental factors: extraction time and temperature, derivatisation time and temperature and pH. The best extraction performance is achieved in the headspace mode, with 5 mL stirred water samples (pH 4) containing 1.3 g of NaCl, equilibrated for 30 min at 25 degrees C, using divinylbenzene-carboxen-polydimethylsiloxane as the fibre coating. On-fibre derivatisation has been used for the first time with 50 microL of bis(trimethylsilyl)trifluoroacetamide at 25 degrees C during 15 min, leading to effective yields. The proposed method provides high sensitivity, good linearity and repeatability (relative standard deviation of 5.1% for 10 ng mL(-1) and n = 5). The limits of detection and quantification were 0.4 and 1.4 ng mL(-1), respectively. Analytical recoveries obtained for different water samples were approx. 100%.

MATERIALS

Product Number

Brand

Product Description

540064

Sigma-Aldrich

(S)-(+)-3-Chloro-1,2-propanediol, 97%, optical purity ee: 97% (GLC)

184489

Sigma-Aldrich

1,3-Dichloro-2-propanol, 97%

107271

Sigma-Aldrich

(±)-3-Chloro-1,2-propanediol, 98%

29534-U

Supelco

Carboxen^® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea

28718-U

Supelco

Tenax^® TA / Carboxen^® 1018, glass TD tube, preconditioned, O.D. × L 1/4 in. × 3 1/2 in., Sealed with (Swagelok^® End-Fittings), pkg of 10 ea

57551-U

Supelco

SPME Fiber Assembly Kit, Assortment, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 4

57286-U

Supelco

SPME Fiber Assembly Kit, Assortment #2, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3

57285-U

Supelco

SPME Fiber Assembly Kit, Assortment #1, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3

57284-U

Supelco

SPME Fiber Assembly Kit, Assortment, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 4

57287-U

Supelco

SPME Fiber Assembly Kit, Assortment #4, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3

57550-U

Supelco

SPME Fiber Assembly Kit, Assortment, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 4

57306

Supelco

SPME Fiber Assembly Kit, Assortment #1, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3

57307

Supelco

SPME Fiber Assembly Kit, Assortment #1, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3

57321-U

Supelco

SPME Fiber Assembly Kit, Assortment #2, Fused Silica (1 cm), size 24 ga, Autosampler, pk of 3

57324-U

Supelco

SPME Fiber Assembly Kit, Assortment #4, Fused Silica (1 cm), size 24 ga, Manual Holder, pk of 3

20355

Supelco

ORBO^™ 78 HBr on Carboxen^® 564 specially cleaned (20/45), 400/200 mg, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea

57325-U

Supelco

SPME Fiber Assembly Kit, Assortment #4, Fused Silica (1 cm), size 24 ga, Autosampler, pk of 3

57320-U

Supelco

SPME Fiber Assembly Kit, Assortment #2, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3

20358

Supelco

ORBO^™ 90 Carboxen^® 564 (20/45), 160/80 mg, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)

57362-U

Supelco

SPME Fiber Assembly Kit, Assortment #5, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 4

32406

Supelco

(±)-3-Chloro-1,2-propanediol, analytical standard

57928-U

Supelco

SPME Fiber Assembly, 100 μm PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, red hub

11048-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 569, 20-45 mesh, bottle of 500 g

54041-U

Supelco

Carboxen^® 1000 Reversible SPE Tube, 200 mg/mL, pk 30

57355-U

Supelco

SPME Fiber Assembly, 60 μm PEG, Metal Alloy (1 cm), needle size 23 ga, Manual Holder, pk of 3, purple hub

57354-U

Supelco

SPME Fiber Assembly, 60 μm PEG, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 3, purple hub

57293-U

Supelco

SPME Fiber Assembly, 65 μm PDMS/DVB, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, pink hub

57345-U

Supelco

SPME Fiber Assembly, 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, blue hub

57294-U

Supelco

SPME Fiber Assembly, 85 μm Polyacrylate, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, white hub

57295-U

Supelco

SPME Fiber Assembly, 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub