Skip to Content
Merck
  • Ultrasound assisted microextraction-nano material solid phase dispersion for extraction and determination of thymol and carvacrol in pharmaceutical samples: experimental design methodology.

Ultrasound assisted microextraction-nano material solid phase dispersion for extraction and determination of thymol and carvacrol in pharmaceutical samples: experimental design methodology.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2014-12-09)
Mostafa Roosta, Mehrorang Ghaedi, Ali Daneshfar, Reza Sahraei
ABSTRACT

In the present study, for the first time, a new extraction method based on "ultrasound assisted microextraction-nanomaterial solid phase dispersion (UAME-NMSPD)" was developed to preconcentrate the low quantity of thymol and carvacrol in pharmaceutical samples prior to their HPLC-UV separation/determination. The analytes were accumulated on nickel sulfide nanomaterial loaded on activated carbon (NiS-NP-AC) that with more detail identified by XRD, FESEM and UV-vis technique. Central composite design (CCD) combined with desirability function (DF) was used to search for optimum operational conditions. Working under optimum conditions specified as: 10 min ultrasonic time, pH 3, 0.011 g of adsorbent and 600 μL extraction solvent) permit achievement of high and reasonable linear range over 0.005-2.0 μg mL(-1) (r(2)>0.9993) with LOD of thymol and carvacrol as 0.23 and 0.21 μg L(-1), respectively. The relative standard deviations (RSDs) were less than 4.93% (n=3).

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetone, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Acetone, ≥99%, meets FCC analytical specifications
Supelco
Acetone, analytical standard
Supelco
Methanol, analytical standard
Sigma-Aldrich
Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
Sigma-Aldrich
Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 30 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME Portable Field Sampler, coating PDMS/DVB
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 30 μm(PDMS, needle size 24 ga, for use with autosampler
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 24 ga, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with manual holder
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), fused silica fiber, df 65 μm(PDMS/DVB, for use with manual holder, needle size 23 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME Portable Field Sampler, coating CAR/PDMS
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with manual holder
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with manual holder, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, for use with autosampler, needle size 23 ga
Supelco
SPME Sampling Stand, for use with 15 mL vials
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Sigma-Aldrich
Sodium phosphate monobasic-16O4, 99.9 atom % 16O
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME Portable Field Sampler, coating PDMS
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 23 ga