A rapid analytical and quantitative evaluation of formaldehyde in squid based on Tri-step IR and partial least squares (PLS).

Formaldehyde abuse for retaining squid freshness is detrimental to public health. The aim is to establish a rapid and quantitative detection method of formaldehyde in squid for screening massive samples. A linear relationship between formaldehyde concentration in squid and formaldehyde concentration in squid soaked water was observed using HPLC. Chemical profile variances of squids were rapidly analyzed by Tri-step infrared spectroscopy. Specifically, with increasing formaldehyde concentration, peak intensities of 2927cm-1 (vas(CH2)), 1081cm-1 (glycogen), 1631cm-1 (ß-sheet proteins) decreased while 1655cm-1 (α-helix proteins) increased. Spectral curve-fitting results further disclosed that ß-sheet proteins were transformed to α-helix and ß-turn conformations. Furthermore, a quantitative prediction model based on IR spectra was established by PLS (R2, 0.9787; RMSEC, 5.51). The developed method was applicable for rapid (c.a. 5min) and quantitative analysis of formaldehyde in squids with LOD of 15mg/kg.

Rapid determination and chemical change tracking of benzoyl peroxide in wheat flour by multi-step IR macro-fingerprinting.

BPO is often added to wheat flour as flour improver, but its excessive use and edibility are receiving increasing concern. A multi-step IR macro-fingerprinting was employed to identify BPO in wheat flour and unveil its changes during storage. BPO contained in wheat flour (<3.0 mg/kg) was difficult to be identified by infrared spectra with correlation coefficients between wheat flour and wheat flour samples contained BPO all close to 0.98. By applying second derivative spectroscopy, obvious differences among wheat flour and wheat flour contained BPO before and after storage in the range of 1500-1400 cm(-1) were disclosed. The peak of 1450 cm(-1) which belonged to BPO was blue shifted to 1453 cm(-1) (1455) which belonged to benzoic acid after one week of storage, indicating that BPO changed into benzoic acid after storage. Moreover, when using two-dimensional correlation infrared spectroscopy (2DCOS-IR) to track changes of BPO in wheat flour (0.05 mg/g) within one week, intensities of auto-peaks at 1781 cm(-1) and 669 cm(-1) which belonged to BPO and benzoic acid, respectively, were changing inversely, indicating that BPO was decomposed into benzoic acid. Moreover, another autopeak at 1767 cm(-1) which does not belong to benzoic acid was also rising simultaneously. By heating perturbation treatment of BPO in wheat flour based on 2DCOS-IR and spectral subtraction analysis, it was found that BPO in wheat flour not only decomposed into benzoic acid and benzoate, but also produced other deleterious substances, e.g., benzene. This study offers a promising method with minimum pretreatment and time-saving to identify BPO in wheat flour and its chemical products during storage in a holistic manner.