Micro(nano)plastics
(MNPs) are widely acknowledged as global environmental
threat while determination methods for MNPs are still lacking and
becoming a growing concern. This study provides a novel method for
MNPs identification/quantification by matrix-assisted laser desorption/ionization–time-of-flight
mass spectrometry (MALDI–TOF MS). Factors affecting the measurement
were optimized, including laser energy, matrix (M), analyte (A), cationization
agent (C), and MAC volume ratio. Under the optimal conditions, the
peaks representative of polystyrene (PS) and polyethylene terephthalate
(PET) were identified, and the mass differences were consistent with
the molecular weight of the corresponding oligomer. A quantitative
correlation was built between normalized signal intensity and ln[polymer
concentration] with a correlation coefficient above 0.96 for low-molecular-weight
polymers and 0.98 for high-molecular-weight polymers. Furthermore,
two types of environmental MNP samples were prepared, including aviation
cup particles as fresh plastics and aged MNPs extracted from river
sediment. By using MALDI–TOF MS, the PS-related MNPs (in both
aviation cup and sediment) consisted of C8H8 and C16H16O oligomers, while the PET-related
MNPs (only found in sediment) were identified with repeated units
of C10H8O4 and C12H12O4. According to the quantitative correlation
curve, the contents of PS and PET MNPs were quantified as 8.56 ±
0.04 and 28.71 ± 0.20 mg·kg–1, respectively,
in the collected sediment. This study is the first attempt to propose
a quantification method with the employment of MALDI–TOF MS
for aged MNPs analysis in environmental samples, which can not only
supply an effective method for MNP analysis but also inspire future
studies on the in situ distribution and transformation of MNPs in
environmental and biological samples.