Determination of alcohol polyether average molar oligomer value/distribution via supercritical fluid chromatography coupled with UV and MS detection

Hoffman, Brian J.; Taylor, Larry T.; Rumbelow, Stephen; Goff, Larry; Pinkston, J. David

doi:10.1016/j.chroma.2004.05.013

Cited by 16 publications

(3 citation statements)

References 27 publications

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“…In addition, a variation of the MS response factors of about two decades is produced when m decreases from 4 to 1 2, 4, 5, 8, and non‐ethoxylated alcohols are not detected 2, 4, 5, 7–9. Several derivatization procedures addressed to add a chromophore or a charge to the oligomers for HPLC and CE 3, 8, 10–15, or to increase volatility for GC 3, 16, 17, have been proposed. Several NP‐ and RP‐HPLC procedures for the characterization of the derivatives using UV–vis 3, 12, 15, 16, 18–20 and MS detection 5, 7, 21–23, have been described.…”

Section: Introductionmentioning

confidence: 99%

Single‐pump bi‐dimensional LC applied to the characterization of derivatized fatty alcohol ethoxylates

Micó-Tormos

Simó‐Alfonso

Ramis‐Ramos

2010

J of Separation Science

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A column selection valve and a 6-port 2-position injection valve were combined to implement bi-dimensional LC in a system driven by a single pump. The system was applied to the separation of linear fatty alcohol ethoxylates with 12-18 carbon atoms in the hydrocarbon moiety, previous derivatization with diphenic anhydride. Separation on the first separation dimension (C(1)) was carried out with a propyl-diol column and an acetonitrile/aqueous ammonium acetate gradient. Fatty alcohol ethoxylate hydrocarbon series (oligomers with the same number of carbon atoms in the alkyl chain but differing in the number of ethylene oxide units) were resolved without distinguishing the oligomers within the series. Selected segments of the eluate of C(1) were transferred to the second column (C(2)), where the successive oligomers within the isolated series were resolved by using either an octyl-silica or a pentafluoro-phenyl-propyl column and an acetonitrile/water gradient. Flow stopping at C(1) during system re-conditioning and elution along the second dimension did not produce any noticeable band broadening. Overlapping of the non-ethoxylated and mono-ethoxylated oligomers with other oligomers within the series was avoided by eluting the pentafluoro-phenyl-propyl column at low temperatures (3 degrees C).

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Section: Introductionmentioning

confidence: 99%

Single‐pump bi‐dimensional LC applied to the characterization of derivatized fatty alcohol ethoxylates

Micó-Tormos

Simó‐Alfonso

Ramis‐Ramos

2010

J of Separation Science

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“…Although this problem was partially resolved through the introduction of refractive index9–12 and evaporative light scattering detection (ELSD) methods,10, 13–17 the limits of detection (LODs) are high for the former, while the sensitivity of ELSD is poor for volatile compounds such as non‐ethoxylated alcohols ( m = 0) and FAE oligomers with a low degree of ethoxylation ( m <3) 18, 19. Finally, low LODs are achieved with chromogenic and fluorogenic pre‐column derivatization procedures 20–38…”

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confidence: 99%

Chromium(VI) oxide oxidation of non‐ethoxylated and ethoxylated alcohols for determination by electrospray ionization mass spectrometry

Beneito‐Cambra

Bernabé-Zafón

Simó‐Alfonso

et al. 2010

Rapid Comm Mass Spectrometry

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A new derivatization procedure to increase the sensitivity of electrospray ionization mass spectrometry (ESI-MS) to non-ethoxylated and ethoxylated alcohols was investigated. The analytes were oxidized with chromium(VI) oxide and the resulting carboxylic and ethoxy-carboxylic acids were isolated by extraction with ethyl acetate; the extracts were alkalinized and infused into the ESI-MS system working in the negative-ion mode. The yields of the combined oxidation-extraction were ca. 100% for non-ethoxylated fatty alcohols dissolved in acetone and they decreased moderately in samples containing increasing amounts of water (e.g., a 75% yield was obtained with 50% water). Ethoxylated alcohols with more than two ethylene oxide units resulted in yields of ca. 60%. Low limits of detection (LODs) were obtained when the procedure was applied to the analysis of body-care products and cosmetics containing fatty alcohols, e.g., in a varicose-vein cream, the LODs were 25 microg cetyl alcohol and 7.5 microg stearyl alcohol (detected as palmitic acid and stearic acid, respectively) per gram of sample. High molecular mass alcohols were also detected in seawater after pre-concentration by solid-phase extraction. Thus, the proposed method is particularly valuable for use in industrial samples having complex matrices and in environmental samples and it is competitive with other methods for the analysis of trace amounts of fatty alcohols.

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“…Like other types of surfactants, the average hydrophile‐lipophile balance (HLB) value of a FAE blend indicates its effectiveness in emulsification and solubilization. In addition, the ability to characterize the average alkyl chain length (m value) and number of EO units (n value) is necessary to determine the HLB of FAEs 3…”

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confidence: 99%

Derivatization of fatty alcohol ethoxylate non‐ionic surfactants using 2‐sulfobenzoic anhydride for characterization by liquid chromatography/mass spectrometry

Praay

Bell

et al. 2009

Rapid Comm Mass Spectrometry

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A derivatization procedure has been developed for the improved characterization of fatty alcohol ethoxylate non-ionic surfactants by liquid chromatography/mass spectrometry. The end hydroxyl group of each surfactant species was converted into an oxycarbonylbenzene-2-sulfonic acid group with 2-sulfobenzoic anhydride under mild conditions. The produced sulfonic acid group allows all species, including fatty alcohols and those with less than three ethoxylates, to be uniformly ionized by electrospray ionization (ESI) mass spectrometry. Both acid and base can be used as a mobile phase additive for liquid chromatography without affecting M(n) and average ethoxylate values, although ion intensities are suppressed during the ESI process. The method was used to analyze seven commercial fatty alcohol ethoxylate non-ionic surfactants, and the determined M(n) and EO values were comparable with the results obtained by NMR. The relative ratio of different fatty alcohol based ethoxylates in a sample can also be determined using the summed mass spectral data.

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Determination of alcohol polyether average molar oligomer value/distribution via supercritical fluid chromatography coupled with UV and MS detection

Cited by 16 publications

References 27 publications

Single‐pump bi‐dimensional LC applied to the characterization of derivatized fatty alcohol ethoxylates

Single‐pump bi‐dimensional LC applied to the characterization of derivatized fatty alcohol ethoxylates

Chromium(VI) oxide oxidation of non‐ethoxylated and ethoxylated alcohols for determination by electrospray ionization mass spectrometry

Derivatization of fatty alcohol ethoxylate non‐ionic surfactants using 2‐sulfobenzoic anhydride for characterization by liquid chromatography/mass spectrometry

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