GCによる製薬の残留溶媒の分析、SPB^®-1 SULFUR、SPME処理、65 μm PDMS/DVB使用

sample/matrix

water + 25% NaCl, pH 11.0 immersion: 3.9 mL sample + 0.1 mL 50% Na3PO4 / 1 g NaCl headspace: 2.4 mL sample + 0.06 mL 50% Na3PO4 / 0.6 g NaCl

SPME fiber

polydimethylsiloxane/DVB, 65 μm (57310-U)

extraction

immersion, 15 min (rapid stirring or headspace, 15 min, 55 °C)

desorption process

270 °C, 5 min

column

SPB-1 SULFUR, 30 m × 0.32 mm I.D., 4.0 μm (24158)

oven

50 °C (2 min) to 180 °C at 10 °C/min

inj. temp.

splitless (3 min), 270 °C (0.75 mm I.D. liner)

detector

FID

carrier gas

helium, 50 cm/sec