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Compatibility of highly sulfated cyclodextrin with electrospray ionization at low nanoliter/minute flow rates and its application to capillary electrophoresis/electrospray ionization mass spectrometric analysis of cathinone derivatives and their optical isomers.
Rapid Commun Mass Spectrom. 2015 Feb 15; 29(3):304-10.RC

Abstract

RATIONALE

Sodium salts of cyclodextrins are commonly used in capillary electrophoresis/mass spectrometry (CE/MS) analysis of illicit drugs and their optical isomers. To avoid the suppression effect of cyclodextrins under electrospray ionization (ESI), the partial filling technique (PFT) is commonly utilized, which has a limited resolution. Low-flow nano-ESI has been shown to reduce the suppression effect of the salts. To test the compatibility of low-flow ESI with a background electrolyte (BGE) containing sodium salts of cyclodextrin, sheathless narrow capillary CE/MS with flow rates of low nanoliters/minute (nL/min) was applied to the separation and detection of cathinones and their positional and optical isomers for the first time.

METHODS

Low-flow sheathless CE/MS using a 20-µm-i.d. capillary in conjunction with a porous tip interface was used for the separation of cathinone derivatives and their optical isomers. Highly sulfated γ-cyclodextrin (HS-γ-CD) in conjunction with (+)-18-crown-6-tetracarboxylic acid ((+)-18-C-6-TCA) was used as the BGE and an ion trap mass spectrometer operating in full scan mode was utilized.

RESULTS

Utilizing low flow rate (~10 nL/min) sheathless CE/MS, the use of the sodium salt of HS-γ-CD as the BGE was compared with the same solution using PFT. The relative and absolute sensitivity of detection of cathinones were about the same, indicating that under low-flow sheathless CE/MS there was no significant suppression due to the existence of HS-γ-CD in the electrospray process. However, enhanced resolution of cathinone derivatives and their positional and optical isomers was observed when the solution of HS-γ-CD was used as the BGE. The enhanced resolution was because of the presence of the HS-γ-CD in the entire capillary during the analysis. The addition of 15 mM (+)-18-C-6-TCA to the BGE containing HS-γ-CD further enhanced the resolution resulting in separation of all cathinones and their positional and optical isomers.

CONCLUSIONS

A novel CE/MS technique has been introduced that combines low-flow sheathless CE/MS, with HS-γ-CD and 15 mM (+)-18-C-6-TCA as the BGE for separation of cathinone derivatives as well as their positional and optical isomers.

Authors+Show Affiliations

Department of Forensic Sciences, George Washington University, Washington, DC, USA.Department of Forensic Sciences, George Washington University, Washington, DC, USA.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

26411628

Citation

Moini, Mehdi, and Christopher M. Rollman. "Compatibility of Highly Sulfated Cyclodextrin With Electrospray Ionization at Low Nanoliter/minute Flow Rates and Its Application to Capillary Electrophoresis/electrospray Ionization Mass Spectrometric Analysis of Cathinone Derivatives and Their Optical Isomers." Rapid Communications in Mass Spectrometry : RCM, vol. 29, no. 3, 2015, pp. 304-10.
Moini M, Rollman CM. Compatibility of highly sulfated cyclodextrin with electrospray ionization at low nanoliter/minute flow rates and its application to capillary electrophoresis/electrospray ionization mass spectrometric analysis of cathinone derivatives and their optical isomers. Rapid Commun Mass Spectrom. 2015;29(3):304-10.
Moini, M., & Rollman, C. M. (2015). Compatibility of highly sulfated cyclodextrin with electrospray ionization at low nanoliter/minute flow rates and its application to capillary electrophoresis/electrospray ionization mass spectrometric analysis of cathinone derivatives and their optical isomers. Rapid Communications in Mass Spectrometry : RCM, 29(3), 304-10. https://doi.org/10.1002/rcm.7106
Moini M, Rollman CM. Compatibility of Highly Sulfated Cyclodextrin With Electrospray Ionization at Low Nanoliter/minute Flow Rates and Its Application to Capillary Electrophoresis/electrospray Ionization Mass Spectrometric Analysis of Cathinone Derivatives and Their Optical Isomers. Rapid Commun Mass Spectrom. 2015 Feb 15;29(3):304-10. PubMed PMID: 26411628.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Compatibility of highly sulfated cyclodextrin with electrospray ionization at low nanoliter/minute flow rates and its application to capillary electrophoresis/electrospray ionization mass spectrometric analysis of cathinone derivatives and their optical isomers. AU - Moini,Mehdi, AU - Rollman,Christopher M, PY - 2014/09/10/received PY - 2014/11/13/revised PY - 2014/11/24/accepted PY - 2015/9/29/entrez PY - 2015/9/29/pubmed PY - 2015/9/29/medline SP - 304 EP - 10 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun. Mass Spectrom. VL - 29 IS - 3 N2 - RATIONALE: Sodium salts of cyclodextrins are commonly used in capillary electrophoresis/mass spectrometry (CE/MS) analysis of illicit drugs and their optical isomers. To avoid the suppression effect of cyclodextrins under electrospray ionization (ESI), the partial filling technique (PFT) is commonly utilized, which has a limited resolution. Low-flow nano-ESI has been shown to reduce the suppression effect of the salts. To test the compatibility of low-flow ESI with a background electrolyte (BGE) containing sodium salts of cyclodextrin, sheathless narrow capillary CE/MS with flow rates of low nanoliters/minute (nL/min) was applied to the separation and detection of cathinones and their positional and optical isomers for the first time. METHODS: Low-flow sheathless CE/MS using a 20-µm-i.d. capillary in conjunction with a porous tip interface was used for the separation of cathinone derivatives and their optical isomers. Highly sulfated γ-cyclodextrin (HS-γ-CD) in conjunction with (+)-18-crown-6-tetracarboxylic acid ((+)-18-C-6-TCA) was used as the BGE and an ion trap mass spectrometer operating in full scan mode was utilized. RESULTS: Utilizing low flow rate (~10 nL/min) sheathless CE/MS, the use of the sodium salt of HS-γ-CD as the BGE was compared with the same solution using PFT. The relative and absolute sensitivity of detection of cathinones were about the same, indicating that under low-flow sheathless CE/MS there was no significant suppression due to the existence of HS-γ-CD in the electrospray process. However, enhanced resolution of cathinone derivatives and their positional and optical isomers was observed when the solution of HS-γ-CD was used as the BGE. The enhanced resolution was because of the presence of the HS-γ-CD in the entire capillary during the analysis. The addition of 15 mM (+)-18-C-6-TCA to the BGE containing HS-γ-CD further enhanced the resolution resulting in separation of all cathinones and their positional and optical isomers. CONCLUSIONS: A novel CE/MS technique has been introduced that combines low-flow sheathless CE/MS, with HS-γ-CD and 15 mM (+)-18-C-6-TCA as the BGE for separation of cathinone derivatives as well as their positional and optical isomers. SN - 1097-0231 UR - https://www.unboundmedicine.com/medline/citation/26411628/Compatibility_of_highly_sulfated_cyclodextrin_with_electrospray_ionization_at_low_nanoliter/minute_flow_rates_and_its_application_to_capillary_electrophoresis/electrospray_ionization_mass_spectrometric_analysis_of_cathinone_derivatives_and_their_optical_isomers_ L2 - https://doi.org/10.1002/rcm.7106 DB - PRIME DP - Unbound Medicine ER -
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