Hydrogen sulfide (H2S), playing unique role on signal transmission in various physiological processes, the rapid and accurate monitoring of it is particularly concerned. The drawbacks of fluorescence probe for H2S, namely poor selectivity or long response time, have always existed. As a test case, here headspace separation combined fluorescence strategy was attempted, on basis of H2S stimuli-responsive AMP/Tb3+/Ag+ or GMP/Tb3+/Ag+ coordination polymer probes. The fluorescence intensity of them is inversely proportional to the concentration of it, due to Ag-S in situ coordination and partial formation of Ag2S. Using the hybrid analysis, a quick response of less than 2.0 min and a high selectivity could be obtained. The signal change (ΔI) of AMP/Tb3+/Ag+ or GMP/Tb3+/Ag+ showed good linearity within the range of 0.5–100 μM and 1.0–150 μM, along with a detection limit (3σ) of 0.2 and 0.4 μM, respectively. When utilized to determine the sulfide level in real samples, it shows recoveries from 96.4 % to 102.3 % with relative standard derivation (RSD) less than 3.0 %. The combination strategy of headspace separation and fluorescence quantitative analysis was verified to effectively eliminate potential interference such as other coexisting non-volatile thiol-containing species, providing a novel avenue to flexibly design the volatile component analysis with high selectivity in complex sample matrixes.
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