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  • Headspace SPME method development for the analysis of volatile polar residual solvents by GC-MS.

Headspace SPME method development for the analysis of volatile polar residual solvents by GC-MS.

Journal of pharmaceutical and biomedical analysis (2000-07-18)
C C Camarasu
ABSTRACT

A solid-phase microextraction (SPME) method has been developed and optimized for the polar residual solvent determination in pharmaceutical products. Five different polymer-coated fibers were investigated and the Carboxen/polydimethylsiloxane was found to be the most sensitive for all components. Two Headspace SPME methods were developed and optimized: one for the extraction from aqueous solutions, and the other for the extraction from organic solutions (N,N-dimethyl formamide (DMF) and dimethyl sulfoxide (DMSO). The optimum equilibration time for all components and all systems was 30 min. It was found that the sample headspace volume has an important effect on method sensitivity and precision. At low headspace volumes (less than one-third of the vial volume), sensitivity improves but at the same time, precision worsens. For 10 ml headspace vials, the optimum headspace volume was found to be 3 ml. The total volatile organic content in the sample also has an important effect on method sensitivity and precision. At low organic content, sensitivity increases but precision drops significantly. Over 0.5% volatile organic content in the sample, the system becomes unstable due to stationary phase swelling by the organic components, and also the sensitivity of the method is drastically reduced. The optimum range for total volatile organic content was found to be between 0.01 and 0.1%. The added Na2SO4 quantity increases the extraction yield. It was found that slightly pressurizing the headspace vial improves the sensitivity of the method by a factor of 2. For the organic system, it was found that the addition of 100 microl DMSO or DMF to 50 mg drug substance and slightly pressurizing the headspace vial gives good results in terms of sensitivity and reproducibility. The measured detection limits were between 0.4 and 200 ng/ml, and the relative standard deviation data were between 2 and 9%. The Headspace SPME from aqueous solutions was found to be ten times more sensitive than Immersion SPME and Headspace SPME from organic solutions.

MATERIALS
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Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
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Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber
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Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
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Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
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Supelco
Headspace vial, screw top, rounded bottom (vial only), volume 20 mL, clear glass vial, thread for 18, O.D. × H 22.5 mm × 75.5 mm, pkg of 100 ea
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
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Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
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Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex
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Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
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Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
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Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
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Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Supelco
Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
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Supelco
Headspace vial, screw top, rounded bottom (vial only), volume 10 mL, clear glass vial, thread for 18, O.D. × H 22.5 mm × 46 mm, pkg of 100 ea
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Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea
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Supelco
ORBO-93 Sorbent Tube, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
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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
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Supelco
Carboxen® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
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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
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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)
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