g-C3N4/Fe3O4 Nanocomposites as Adsorbents Analyzed by UPLC-MS/MS for Highly Sensitive Simultaneous Determination of 27 Mycotoxins in Maize: Aiming at Increasing Purification Efficiency and Reducing Time.

According to known studies, numerous mycotoxins have been found simultaneously in foods and have a certain expansion toxicity, so the simultaneous detection of multiple mycotoxins is absolutely critical. In this article, multifunctional magnetic g-C3N4/Fe3O4 nanocomposites have been fabricated to employ as modified QuEChERS adsorbents. In addition, they were also used in conjunction with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), an accurate quantitative approach, to analyze 27 mycotoxins in maize. The improved method not only has a powerful adsorption effect on the complex matrix by g-C3N4/Fe3O4 but also enables magnetic separation from the sample solution. Experiments proved that this method can exhibit good linearity under the appropriate and optimal external environment (r2 ≥ 0.9954), high sensitivity (the threshold of detection limit is 0.0004-0.6226 µg kg-1, and the threshold of quantification limit is 0.0014-2.0753 µg kg-1), adequate recoveries (77.81-115.21%), and excellent repeatability (with a threshold of intraday precision of 1.5-10.8% and interday precision in the range of 2.9-12.5%). In practice this method has been used to evaluate a variety of mycotoxins in maize specimens, and certain actual outcomes have been achieved.

[Research on Rapid and Non-Destructive Identification of Aging Wheat Based on ATR-Terahertz Spectroscopy Combined with PLS-DA].

In this research, the terahertz spectra data of the aging wheat processed under manual control environment by ATR accessory were collected. After the data diversity based on the composite score by PCA, the non-destructive identification models of aging wheat were developed by PLS-DA algorithm. The results showed that for the absorption coefficient spectrum, the accuracy of the experimental group, control group of the calibration set and cross validation set were 84.2%, 94.7%, 84.2% and 81.6% respectively, while the accuracy of the experimental group and control group of the external validation set were 73.7% and 100.0% respectively; for the refractive index spectrum, the accuracy of the experimental group, control group of the calibration set and cross validation set were 84.2%, 92.0%, 76.3% and 76.3% respectively, while the accuracy of the experimental group and control group of the external validation set were 84.2% and 89.5% respectively. The research indicates that ATR-THz technology should be of great potentials in the application in the non-destructive identification of aging wheat.

Statistical analysis of sudden chemical leakage accidents reported in China between 2006 and 2011.

According to the data from authoritative sources, 1,400 sudden leakage accidents occurred in China during 2006 to 2011 were investigated, in which, 666 accidents were used for statistical characteristic abstracted with no or little damage. The research results were as follows: (1) Time fluctuation: the yearly number of sudden leakage accidents is shown to be decreasing from 2006 to 2010, and a slightly increase in 2011. Sudden leakage accidents occur mainly in summer, and more than half of the accidents occur from May to September. (2) Regional distribution: the accidents are highly concentrated in the coastal area, in which accidents result from small and medium-sized enterprises more easily than that of the larger ones. (3) Pollutants: hazardous chemicals are up to 95 % of sudden leakage accidents. (4) Steps: transportation represents almost half of the accidents, followed by production, usage, storage, and discard. (5) Pollution and casualties: it is easy to cause environmental pollution and casualties. (6) Causes: more than half of the cases were caused by human factor, followed by management reason, and equipment failure. However, sudden chemical leakage may also be caused by high temperature, rain, wet road, and terrain. (7) The results of principal component analysis: five factors are extracted by the principal component analysis, including pollution, casualties, regional distribution, steps, and month. According to the analysis of the accident, the characteristics, causes, and damages of the sudden leakage accident will be investigated. Therefore, advices for prevention and rescue should be acquired.

[Reason analysis of inadaptability and its correction research on the authenticity identification model of West Lake Longjing tea based on LVF micro-NIR spectrometer].

In the present paper, the micro-NIR spectrometer with the splitter of linear variable filter was used to develop the recognition models of the West Lake Longjing tea and the ordinary flat tea of the year 2012 and 2013. The NIR spectral data of different years and different storage times were decomposed by PCA algorithm. The PLS-DA models were developed by the representative samples selected by the mathematical characteristics of PCA-scores' distribution in order to analyze the reason for the inadaptability of the models according to mathematical principles and find out the solution for its correction. Being examined by the external validation set, the adaptability of the authenticity identification model was enhanced effectively. The result of this research indicated that, for the West Lake Longjing tea and the ordinary flat tea, the correct recognition rate of the model developed by all different-year samples' NIR spectral data would be enhanced effectively. The model developed by the NIR spectral data of different storage time samples indicated that the physicochemical properties of the ordinary flat tea have changed remarkably after cryopreservation for 3 months, while the physicochemical properties of the West Lake Longjing tea are relatively stable. The model adaptabilities for different years and different storage times were studied according to the mathematical perspective of the principal component characteristics of spectral data. After the authenticity identification model of West Lake Longjing tea was developed, the prediction accuracy was enhanced effectively. This research would provide reference for not only the application of NIR spectroscopy in quality grading and safety of agricultural products, but also the enhancement of the prediction accuracy of the NIR grading models for agricultural products.

[Research on the quantitative determination of lime in wheat flour by near-infrared spectroscopy].

The safety of wheat flour is always focused by all quarters of society. Based on comparing the feature of NIR spectra of calcium oxide, calcium hydroxide and calcium carbonate in this research, the diffuse reflection NIR spectra of the wheat flour samples with different content of calcium oxide, calcium hydroxide and calcium carbonate mixed in were collected. The calibration models of lime and calcium carbonate were developed by partial least square algorithm, with the validation method of cross validation. The result indicated that the determination coefficients (R2) of lime and calcium carbonate are 99.80% and 96.98% respectively, the root mean square errors of calibration set are 0.19 and 0.34 respectively; the root mean square errors of cross validation set are 0.26 and 0.75 respectively; the root mean square errors of prediction set are 0.63 and 0.44 respectively; the ratio performance deviations (RPD) are 8.57 and 5.24 respectively, which indicated that the calibration models were precise enough to adapt to the on-site rapid determination of lime in wheat flour. The result of F-test indicated that a very remarkable correlation exists between the estimated and specified values of the calibration sets and the external validation sets. This research, to some extent, will provide some reference methods for the rapid determination of wheat flour for quality safety, which is important for the quality control of wheat flour.

[Analysis of heavy metal in soil with portable X-ray fluorescence spectrometry].

The concentrations of main heavy metal pollutants (Cu, Zn, Pb, Cr and As) in soil were tested by NITON XL3 600 portable X-ray fluorescence spectrometry (PXRF). The results showed that the minimum? detection limits for elements Cu, Zn, Pb, Cr and As were 23.96, 11.69, 8.58, 19.23, 6.24 mg x kg(-1), respectively. The soil composition standard material GSS-5 was detected by PXRF for 5 replicate measurements, The accuracy was 96%-102% and relative standard deviations (RSD) was 1.0%-7.6%. In term of field situ testing, RSD was less than 20%, and accuracy was 55%-119%. The performance was assessed by laboratory testing and field situ detection, and the results indicated that PXRF is effective for rapid, quantitative monitoring of soil metal contamination.

[FTIR microspectroscopy and its progress in application].

FTIR microspectroscopy technique was born in the mid-nineties. The research on this technique has just began abroad, and this technology has not yet been widely recognized in China. It is a rapid, nondestructive testing technology, has the advantages of microdomain, visualization, high precision and high sensitivity. In the present study, the composition, operational principle and working mode of FTIR microspectroscopy were summarized. The progress in application of FTIR microspectroscopy technique was investigated in some fields, including biomedicine, microbiology, forensic science, materials science, nutrition and feed science and agricultural products. The difficulty of FTIR microspectroscopy research and the prospects of this technique were also discussed.

[Comparative research on the NIR and MIR micro-imaging of two similar plastic materials].

The NIR/MIR micro-imaging can supply not only the information of spectra, but also the information of spacial distribution of the sample, which is superior to the traditional NIR/MIR spectroscopy analysis. In the present paper, polyethylene and parafilm, with similar appearances, were regarded as the research objects, of which the NIR/MIR micro-imaging was collected. Chemical imaging (CI) and compare correlation imaging were carried out for the two materials respectively to discuss the imaging methods of the two materials. The result indicated that the differentiation of the CI values of the two materials in the NIR/MIR CI for material II was 0.004 8 and 0.254 8 respectively, while those in the NIR/MIR CI for material I were 0.002 6 and 0.326 5, respectively. Clear CI was acquired, and the two materials could be differentiated. The result of the compare correlation imagings indicated that the compare correlation imagings, in which the NIR/MIR spectra of the two materials were regarded as reference spectra respectively, can differentiate the two materials remarkably with clear imagings. In the compare correlation imagings of MIR micro-imaging, the difference of the correlation coefficients between the two materials' MIR spectra and the reference spectrum was more than 0.12, which showed a better imaging result; while a tiny difference of the correlation coefficients between the two materials' NIR spectra and the reference spectrum could be employed to show a clear imaging result for NIR compare correlation imaging so as to differentiate the two materials. This thesis, to some extent, can supply the reference to not only the rapid discrimination of the safety of the packaging material for agri-food, but also the imaging methods for NIR/MIR micro-imaging to differentiate the different materials.

[Determination of Cr, Cu, Zn, Pb and As in soil by field portable X-ray fluorescence spectrometry].

Total concentrations of Cr, Cu, Zn, Pb and As were determined in soil samples from Beijing, Xinjiang, Heilongjiang, Yunnan, and Jiangsu provinces, using field portable X-ray fluorescence spectrometry (XRF). The relationship between XRF analysis results and the concentration of heavy metals in soils was established. The influence of soil particle size and humidity was also considered. Experiments showed that the particle size of soil affected XRF performance. While particle size decreased from 420 to 180 microm, the relative standard deviation (RSD) of XRF detect results reduced from 15.6% to 6.9%. Soil humidity mainly affected the counts of XRF measured. As the soil water content increased from 5% to 252, the analysis result's relative ratio of humid soil samples to oven dried soil samples decreased from 86% to 69%, according with the equation I = 100e(0.015c), where I means relative ratio, and c means water content (R2 = 0.83, n=30). A high degree of linearity was found for all the five heavy metals with the XRF measurement in the range of 0 to 1500 mg x kg(-1). But the linearity equation was not the same among these soils. The linearity equation established with Yunnan soil has a small slope because of higher Fe concentration in soil. The performance of instrument was assessed by comparing XRF analysis result with the standard sample reference, and the result showed that XRF is an effective tool for rapid, quantitative monitoring of soil metal contamination.

Development of an enzyme-linked immunosorbent assay for podophyllotoxin.

A competitive indirect enzyme-linked immunosorbent assay (ciELISA) for podophyllotoxin was developed by using polyclonal antibody, and its suitability for the determination of this analyte in spiked water samples was studied. To avoid antibody production to the linker, the succinoyl-podophyllotoxin (hapten) mimicking the analyte was synthesized and conjugated with the carrier proteins bovine serum albumin (BSA) and ovalbumin (OVA) by mixed anhydride reaction (MAR) and active ester method (AEM). Polyclonal antibodies raised against Hapten-BSA(1) synthesized by MAR and Hapten-BSA(2) by AEM were screened and selected for the ciELISA. One set of antibodies from the rabbit M4440 immunized with Hapten--BSA(1) showed an I(50) value of 2.21 microg/mL with a detection limit of 0.12 microg/mL, and the other set from the rabbit M4469 immunized with Hapten-BSA(2) had an I(50) value of 0.7897 microg/mL with a detection limit of 0.0056 microg/mL. This assay showed the cross-reactivities with the structurally closely related compounds. Recoveries from the podophyllotoxin-fortified tap water in the assay were in the range of 72--115%. A good correlation between podophyllotoxin concentration measured by the ELISA and HPLC (R(2)=0.9924, Y=1.195X-0.257) was obtained from linear regression analysis. These results indicate that the ELISA could be a convenient and supplemental analytical tool for monitoring podophyllotoxin and its analogues in waters without previous extraction or cleanup.