Influence of ionic strength and organic modifier on performance in capillary electrochromatography on phenyl silica stationary phase

An isocratic elution pressurized CEC (pCEC) system was used to separate and determine ten carbamate insecticides. It was found that introduction of the electrical field, supplementary pressure, and SDS in the proposed method greatly improved the speed, column efficiency, selectivity, and repeatability for separation and determination of carbamates. On a capillary column of 75 microm ID packed with 3 microm octadecyl silica, baseline separation and detection of ten analytes was performed by using a mobile phase consisting of 30% v/v ACN and 70% v/v of 5 mmol/L ammonium acetate (pH 6.5) containing 1 mmol/L SDS and 0.01% triethylamine (TEA). Under the optimum conditions ten carbamate insecticides could be completely separated within 20 min. For the real vegetable samples, an SPE procedure for the cleanup of matrices was carried out prior to pCEC analysis. The detection limits of 0.05-1.6 mg/kg for ten carbamates and mean recoveries of 51.3-109.2% for eight kinds of vegetable samples at different concentrations of carbamates with RSD less than 11.4% were obtained, respectively. The proposed method has been proved to be effective in the rapid analysis of carbamate residues in vegetables.

Section: Optimization Of the Separation And Determination Conditions supporting

confidence: 76%

Rapid separation and determination of carbamate insecticides using isocratic elution pressurized capillary electrochromatography

Ling

Xie

et al. 2006

“…Resolution was also significantly improved with the decrease in ACN concentration. This was due to the increase in the hydrophobic interaction between the analyte and the CSP as a result of decreasing ACN concentration [36].…”

Section: Effect Of Different Compositions Of Organic Modifiermentioning

confidence: 99%

Application of Click‐chemistry‐based perphenylcarbamated β‐CD chiral stationary phase in CEC

Wang¹,

Xiao²,

Tan³

et al. 2009

A novel chiral stationary phase (CSP) was prepared by anchoring mono-6-azido-6-deoxyperphenylcarbamated beta-CD onto omega-alkynyl functionalized silica (5 microm) via organic soluble Cu(I)-catalyzed Click chemistry. The obtained CSP was thereafter packed into fused-silica capillary (100 microm id) with an effective length of 9 cm and tested in aqueous CEC to separate a series of racemic aryl alcohols. High separation factors with good resolution were achieved using the current novel CSP. Some pharmaceutical compounds could also be well resolved on this newly derived CSP. The analytical results demonstrate that Click-chemistry-based perphenylcarbamated CSP affords high stability in high electric field and depicts excellent enantioseparation in CEC. The effects of pH value, buffer concentration, applied voltage, concentration of organic modifier and analyte structure on the enantioseparation are also discussed.

“…This technique has been shown to be suitable for the separation of benzodiazepines [23][24][25][26]. There are several solutions to the problem of introducing a stationary phase into a fused-silica capillary.…”

Section: Introductionmentioning

confidence: 99%

Determination of trace levels of benzodiazepine in urine using capillary electrochromatography‐time of flight mass spectrometry

Blas

McCord

2008

This paper details a method for the separation and determination of ten benzodiazepines in urine using CEC-MS(TOF) and an hexyl acrylate-based porous monolith. The TOF mass spectrometer provides an exact mass of protonated benzodiazepines to three decimal places (1-6 ppm). This high selectivity along with the CEC separation, provides an effective method for the identification of benzodiazepines. Linearity is satisfactory for all compounds in the concentration range of 25-500 ng/mL for lorazepam and 12.5-500 ng/mL for the others. The RSDs are between 1.4-2.3% for retention times and 1.1-9.2% for relative areas. Using the monolithic stationary phase, a preconcentration step is achievable and permits an 75-140-fold improvement in sensitivity. This strategy permits the quantification of these drugs down to 1 ng/mL in urine. This method was used for the analysis of benzodiazepines in spiked urine samples.