Automated needle-sleeve based online hyphenation of solid-phase microextraction and liquid chromatography

Area of Science:

• Analytical Chemistry
• Environmental Science

Background:

• Estrogen-like isoflavones are important biomarkers in human urine.
• Existing microextraction techniques face challenges like clogging and dispersion.
• Online coupling of extraction and chromatography offers efficiency gains.

Purpose of the Study:

• To develop and validate a novel automated online SPME-LC-UV method.
• To determine estrogen-like isoflavones in human urine samples.
• To address limitations of current graphene-based microextraction techniques.

Main Methods:

• Development of a Si@GO@βCD coated needle-sleeve extractant device.
• Online coupling of SPME with LC using a lab-made autosampler.
• Direct immersion extraction, rinsing, desorption/enrichment, and online transfer to LC.

Main Results:

• The method achieved good sensitivity with detection limits as low as 10 μg/L.
• High reliability was demonstrated with intra-day RSD <10% and inter-day RSD <13%.
• The total analysis time was reduced to under 17 minutes per sample.

Conclusions:

• The automated online SPME-LC method provides a sensitive, reliable, and straightforward strategy.
• This approach effectively determines organic compounds in complex matrices like human urine.
• The developed technique overcomes drawbacks of traditional graphene-based microextraction methods.