Impacto da irradiação com laser ND: YAG sobre primer de adesivo convencional na adesão à dentina / Impact of Nd: YAG laser irradiation on primer of conventional adhesive in adhesion to dentin

A irradiação da dentina com o laser Nd:YAG mostra-se promissora para a qualidade da adesão, desde que aplicada sob parâmetros específicos e em etapas definidas. O objetivo deste estudo é avaliar de forma comparativa, o impacto da irradiação com laser de Nd:YAG sobre a formação e estabilidade da camada híbrida em dentina humana, pré-tratada com ácido e primer de sistema adesivo convencional, "in vitro". Setenta molares hígidos tiveram suas raízes e porções coronárias seccionadas horizontalmente, até completa exposição de dentina oclusal. As amostras foram divididas em: G1 (controle n=20); G2 (experimental n=20), sendo 10 dentes de cada grupo destinados ao microcisalhamento (MC) e 10 dentes à microscopia eletrônica de varredura (MEV). Nos 30 dentes restantes analisou-se: textura por Tomografia Computadorizada de Feixe Cônico (AT=15); e Espectroscopia de Infravermelho por Transformada de Fourier (FTIR=15) em 3 momentos: dentina controle; após tratamento com ácido + primer; e posterior à irradiação a laser. Estatisticamente, optou-se por ANOVA 1 fator, Qui Quadrado de Pearson, teste T e múltiplas comparações de Tukey com significância de 5%. A FTIR evidenciou redução dos níveis de fosfato e carbonato nos momentos primer e após irradiação laser, porém não havendo desnaturação do colágeno exposto. A análise de textura evidenciou uma tendência à formação de um tecido mais padronizado após o uso do laser. O teste de MC evidenciou valores médios de 36,5 e 35,2MPa para G1 e G2 respectivamente (p>0,05) e portanto, de forma imediata, o laser não mostrou efeitos deletérios ao processo adesivo. Além disso, observou-se maior penetrabilidade do adesivo na avaliação em MEV após a aplicação do laser. Novas pesquisas com avaliação longitudinal mostram-se necessárias para verificar se o efeito do laser pode ter sido protetor da degradação hidrolítica, visto que há uma redução do conteúdo de água local durante a formação da camada híbrida (AU).

Irradiation of dentin with the Nd:YAG laser shows promise for the quality of adhesion, as long as it is applied under specific parameters and in defined steps. The objective of this study is to comparatively evaluate the impact of irradiation with Nd:YAG laser on the formation and stability of the hybrid layer in human dentin, pretreated with acid and primer of conventional adhesive system, "in vitro". Seventy healthy molars had their roots and coronal portions horizontally sectioned, until complete exposure of occlusal dentin. The samples were divided into: G1 (control n=20); G2 (experimental n=20), with 10 teeth from each group destined for microshearing (MC) and 10 teeth for scanning electron microscopy (SEM). In the 30 remaining teeth analyzed: texture by Cone Beam Computed Tomography (AT=15); and Fourier Transform Infrared Spectroscopy (FTIR=15) in 3 moments: dentin control; after treatment with acid + primer; and after laser irradiation. Statistically, we opted for 1-way ANOVA, Pearson's Chi Square, T test and Tukey's multiple comparisons with a significance of 5%. FTIR showed a reduction in phosphate and carbonate levels in the primer moments and after laser irradiation, but there was no denaturation of the exposed collagen. The texture analysis evidenced a trend towards the formation of a more expressive tissue after the use of the laser. The CM test showed mean values of 36.5 and 35.2MPa for G1 and G2 respectively (p>0.05) and therefore, immediately, the laser showed no deleterious effects on the adhesive process. In addition, greater penetrability of the adhesive was observed in the SEM evaluation after laser application. New studies with longitudinal evaluation are necessary to verify if the laser effect could have been protected from hydrolytic degradation, since there is a reduction in the local water content during the formation of the hybrid layer (AU).

Analysis of Olibanum and Myrrha by Differential Scanning Calorimetry and Fourier Transform InfraRed / 国际中医中药杂志

Objective:To distinguish the differences between Olibanum and Myrrha by using modern analytical methods such as Differential Scanning Calorimeter (DSC) and Fourier Transform InfraRed (FT-IR). Methods:By collecting Olibanum and Myrrha in different growing areas and different processed prosecures, this paper to analizes the influence of temperature increase and its speed , as well as the particle size on the DSC experiment. The DSC method was used to perform a differential thermal map of Olibanum and Myrrha scanning and analysis; FT-IR was used to scan and analyze 20 batches of Olibanum and Myrrha. Results:TThe results of DSC analysis showed that the DSC experimental condition ranged between 30-600 ℃; the speed of temperature increase was 30 ℃/min; the particle size was 100 mesh. The DSC spectra of of Olibanum and Myrrha were significantly different. Only the processed products of frankincense had endothermic peak near 297 ℃, and there was no characteristic peak in this temperature range. Their exothermic peaks are close at 326 ℃, but their enthalpy values are quite different. The position of endothermic peak near 100 ℃ is close to the size of peak shape. FT-IR test showed that the absorption peaks of Olibanum and Myrrha at wave numbers 2 925, 1 710, 1 454, 1 371, 1 242, 1 029 cm -1 appeared, and the positions of strong peaks were also similar. The intensity of the characteristic peak of Myrrha wave number 1 029 cm -1 is greater than that of Olibanum. Conclusion:The DSC spectra of Olibanum and Myrrha are significantly different, and the difference between the two FT-IR spectra is small. Differential scanning Calorimetry is an effective, fast, and simple way to identify resinous Chinese medicinal materials, and is worthy of further popularization.

The influence of the particle's size on the setting reaction of sol-gel derived calcium silicate particles / A influência do tamanho de partícula na reação de presa de cimentos de silicate de cálcio produzidos por sol-gel

Introduction: This study aims to analyze the influence of particles size of sol-gel derived calcium silicate particles in the setting reaction of bioactive endodontic cements. Materials and Methods: Sol-gel derived calcium silicate particles were synthesized and sieved to separate the particles in different sizes: CS400, CS200, and CS100. A commercial MTA (Control) was used as control. The particle size and the specific surface area were assessed by laser diffraction and nitrogen adsorption. The cements were prepared with water as the liquid for the reaction. The setting time was conducted according to ISO 6876, and the setting kinetics was analyzed by Fourier trans-formed infrared spectroscopy (FTIR) at different time points between 120s to 72h. Results: The particle size varied from 9.45µm (CS400 ) to 31.01 (Control). The higher specific surface area valuer reached 15.14g/cm2 in the CS400. The smallest particle sizes, the higher specific surface area, and the lowest setting time were found for CS400 (p < 0.05). Control presented the highest setting time (p < 0.05). The FTIR analyses showed the differences in materials structure over time, with faster hydration and crystallization for CS400. The setting kinetics was slower for Control even when compared to a sol-gel derived group with similar particle size. Conclusion:The route of synthesis and the particle size influences the setting reaction of calcium silicate-based cements. The reduction of particle size for sol-gel derived calcium silicates lead to the acceleration of the setting reaction of the produced bioactive endodontic cement.

Introdução: Este estudo tem como objetivo analisar a influência do tamanho de partículas de silicato de cálcio derivadas de sol-gel na reação de presa de cimentos endodônticos bioativos. Materiais e Métodos: Partículas de silicato de cálcio derivadas de sol-gel foram sintetizadas e peneiradas para separar as partículas em diferentes tamanhos: CS400, CS200 e CS100. Um MTA comercial (Controle) foi usado como controle. O tamanho das partículas e a área superficial específica foram avaliados por difração a laser e adsorção de nitrogênio. Os cimentos foram preparados com água como líquido para a reação. O tempo de presa foi conduzido de acordo com a ISO 6876, e a cinética de presa foi analisada por espectroscopia de infravermelho transformada de Fourier (FTIR) em diferentes pontos de tempo entre 120s a 72h. Resultados: O tamanho de partícula variou entre 9,45µm (CS400) e 31,01 (Controle). A maior área de superfície foi encontrada nas partículas do grupo CS400 (15.14g/cm2). Os menores tamanhos de partícula, a maior área de superfície específica e o menor tempo de presa foram encontrados para CS400 (p < 0,05). O Control apresentou o maior tempo de presa (p < 0,05). As análises de FTIR mostraram as diferenças na estrutura dos materiais ao longo do tempo, com hidratação e cristalização mais rápidas para CS400. A cinética de presa foi mais lenta para Control mesmo quando comparado a um grupo derivado de sol-gel com tamanho de partícula semelhante. Conclusão: A rota de síntese e o tamanho das partículas influenciam a reação de endurecimento dos cimentos à base de silicato de cálcio. A redução do tamanho de partícula para silicatos de cálcio derivados de sol-gel leva à aceleração da reação de pega do cimento endodôntico bioativo produzido.

Rapid Qualitative and Quantitative Analysis of Caffeine and Sodium Benzoate in Annaca by Infrared Spectroscopy.

ABSTRACT: Objective To establish an infrared spectroscopic method for the rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples. Methods Qualitative and quantitative modeling samples were prepared by mixing high-purity caffeine and sodium benzoate. The characteristic absorption peaks of caffeine and sodium benzoate in Annaka samples were determined by analyzing the infrared spectra of the mixed samples. The quantitative model of infrared spectra was established by partial least squares （PLS）. Results By analyzing the infrared spectra of 17 mixed samples of caffeine and sodium benzoate （the purity of caffeine ranges from 10% to 80%）, the characteristic absorption peaks for caffeine were determined to be 1 698, 1 650, 1 237, 972, 743, and 609 cm-1. The characteristic absorption peaks for sodium benzoate were 1 596, 1 548, 1 406, 845, 708 and 679 cm-1. When the detection of all characteristic absorption peaks was the positive identification criteria, the positive detection rate of caffeine and sodium benzoate in 48 seized Annaka samples was 100%. The linear range of PLS quantitative model for caffeine was 10%-80%, the coefficient of determination （ R2） was 99.9%, the root mean square error of cross validation （RMSECV） was 0.68%, and the root mean square error of prediction （RMSEP） was 0.91%; the linear range of PLS quantitative model for sodium benzoate was 20%-90%, the R2 was 99.9%, the RMSECV was 0.91% and the RMSEP was 1.11%. The results of paired sample t test showed that the differences between the results of high performance liquid chromatography method and infrared spectroscopy method had no statistical significance. The established infrared quantitative method was used to analyze 48 seized Annaka samples, the purity of caffeine was 27.6%-63.1%, and that of sodium benzoate was 36.9%-72.3%. Conclusion The rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples by infrared spectroscopy method could improve identification efficiency and reduce determination cost.

Rapid Qualitative and Quantitative Analysis of Caffeine and Sodium Benzoate in Annaca by Infrared Spectroscopy / 法医学杂志

Objective To establish an infrared spectroscopic method for the rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples. Methods Qualitative and quantitative modeling samples were prepared by mixing high-purity caffeine and sodium benzoate. The characteristic absorption peaks of caffeine and sodium benzoate in Annaka samples were determined by analyzing the infrared spectra of the mixed samples. The quantitative model of infrared spectra was established by partial least squares （PLS）. Results By analyzing the infrared spectra of 17 mixed samples of caffeine and sodium benzoate （the purity of caffeine ranges from 10% to 80%）, the characteristic absorption peaks for caffeine were determined to be 1 698, 1 650, 1 237, 972, 743, and 609 cm-1. The characteristic absorption peaks for sodium benzoate were 1 596, 1 548, 1 406, 845, 708 and 679 cm-1. When the detection of all characteristic absorption peaks was the positive identification criteria, the positive detection rate of caffeine and sodium benzoate in 48 seized Annaka samples was 100%. The linear range of PLS quantitative model for caffeine was 10%-80%, the coefficient of determination （ R2） was 99.9%, the root mean square error of cross validation （RMSECV） was 0.68%, and the root mean square error of prediction （RMSEP） was 0.91%; the linear range of PLS quantitative model for sodium benzoate was 20%-90%, the R2 was 99.9%, the RMSECV was 0.91% and the RMSEP was 1.11%. The results of paired sample t test showed that the differences between the results of high performance liquid chromatography method and infrared spectroscopy method had no statistical significance. The established infrared quantitative method was used to analyze 48 seized Annaka samples, the purity of caffeine was 27.6%-63.1%, and that of sodium benzoate was 36.9%-72.3%. Conclusion The rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples by infrared spectroscopy method could improve identification efficiency and reduce determination cost.

Efeito de diferentes protocolos de colagem de bráquetes cerâmicos com LED de alta potência / Effect of different ceramic bracket bonding protocols with high power LED

OBJETIVO: Avaliar o efeito de diferentes protocolos de fotoativação na resistência de união ao cisalhamento (RUC) de bráquetes cerâmicos colados ao esmalte dentário, nas falhas de união através do índice remanescente adesivo (IRA) e no grau de conversão (GC) de uma resina utilizando o fotoativador de alta potência Valo™ Cordless® (Ultradent) no modo Xtra power (3.200 mW/cm2 ). METODOLOGIA: Os bráquetes foram colados (Transbond XT® , 3M Unitek) em 80 coroas de incisivos bovinos, distribuídas aleatoriamente em dois grupos (N=40): bráquetes monocristalinos (Grupo 1) e bráquetes policristalinos (Grupo 2). Cada grupo foi subdividido em 4 subgrupos (n=10) de acordo com o protocolo de fotoativação: 3 ou 6 segundos no centro; 3s na mesial/3s na distal; e 3s na cervical/3s na incisal. Após armazenamento por 4 meses (água destilada/37°C), realizou-se o ensaio de cisalhamento (100KgF, 1mm/min). Para análise do GC, foram confeccionados 80 discos de resina com os mesmos protocolos de fotoativação utilizados na colagem dos bráquetes. A RUC (MPa) foi avaliada descritivamente, pelo teste T de Student, ANOVA one- e two-way e pelo pós-teste de Tukey. O GC (%) foi avaliado descritivamente, pela ANOVA two-way e pelo pós-teste de Tukey. As falhas de união foram classificadas de acordo com o IRA, analisadas descritivamente e pelo teste de KruskalWallis. RESULTADOS: Em relação à RUC, todos os protocolos do Grupo 2 e apenas o de fotoativação no centro por 3 segundos do Grupo 1 apresentaram valores clinicamente aceitos; os valores foram significativamente afetados (p<0,01) pelo tipo de bráquete; e ao comparar as médias intergrupos correspondentes, observou-se p=0,003 entre os protocolos de 6s no centro e p=0,010 entre os protocolos de 3s na cervical/3s na incisal. Na avaliação do GC, os valores foram afetados de forma estatisticamente significativa pelo protocolo de fotoativação (p=0,002) e pela interação entre os fatores (tipo de bráquete*protocolo de fotoativação; p=0,033). Os escores 4 (39,4%; p>0,05) e 3 (72,5%; p=0,001) do IRA foram predominantes nos Grupos 1 e 2, respectivamente. CONCLUSÃO: Deve-se ter cautela ao realizar a colagem de bráquetes cerâmicos com o Valo™ Cordless® no modo Xtra power, pois observou-se RUCs altas. A RUC e o GC podem apresentar diferenças estatisticamente significativas a depender do tipo de bráquete e do protocolo de fotoativação aplicado. De modo geral, sugere-se utilizar o bráquete policristalino ao monocristalino e aplicar 3 segundos de fotoativação no centro do bráquete (AU).

OBJECTIVE: To evaluate the effect of different photoactivation protocols on shear bond strength (SBS) of ceramic brackets bonded to dental enamel, on bond failure through the adhesive remnant index (ARI) and on the degree of conversion (DC) of a resin using the highpower photo activator Valo™ Cordless® (Ultradent) in Xtra power mode (3.200 mW/cm2 ). METHODOLOGY: The brackets were bonded (Transbond XT® , 3M Unitek) on 80 crowns of bovine incisors, randomly distributed into two study groups (N=40): monocrystalline brackets (Group 1) and polycrystalline brackets (Group 2). Each group was subdivided into 4 subgroups (n=10) according to the photoactivation protocol used: 3 or 6 seconds in the center; 3s in the mesial/3s in the distal; and 3s in the cervical/3s in the incisal. After storage for 4 months (distilled water/37°C), the shear test (100KgF, 1mm/min) was performed. For DC analysis, 80 resin discs were made with the same photoactivation protocols used in bonding brackets. The SBS (MPa) was evaluated descriptively, using Student's T test, ANOVA one- and two-way and by Tukey's post-test. The DC (%) was assessed descriptively, by ANOVA two-way and by Tukey's post-test. Union failures were classified according to the ARI, analyzed descriptively and by Kruskal-Wallis' test. RESULTS: Regarding the SBS, all protocols in Group 2 and only the photoactivation on the center for 3 seconds of Group 1 presented clinically accepted values; the values were significantly affected (p<0.01) by the type of bracket; and when comparing the corresponding intergroup averages, p=0.003 was observed between the protocols of 6s in the center and p=0.010 between the protocols of 3s in the cervical/3s in the incisal. In the DC evaluation, the values were significantly affected by the photoactivation protocol (p=0.002) and by the interaction between the factors (type of bracket*photoactivation protocol; p=0.033). ARI scores 4 (39.4%; p>0.05) and 3 (72.5%; p=0.001) were predominant in Groups 1 and 2, respectively. CONCLUSION: Caution should be exercised when bonding ceramic brackets with Valo™ Cordless® in Xtra power mode, because high SBSs were observed. SBS and DC might present statistically significant differences depending on the type of bracket and the photoactivation protocol applied. In general, it is suggested to use the polycrystalline bracket to the monocrystalline and apply 3 seconds of photoactivation in the center of the bracket (AU).

[Structure Analysis and Characterization of Aminorex Analogue 4'-F-4-MAR].

ABSTRACT: Objective To study the identification method for 4'-F-4-methylaminorex （4'-F-4-MAR） in samples without reference substance. Methods Gas chromatography-mass spectrometry （GC-MS）, ultra-high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry （UPLC-QTOF-MS）, nuclear magnetic resonance （NMR） and Fourier transform infrared （FTIR） were comprehensively used for the structure identification of 4'-F-4-MAR in samples. Results Under the positive electrospray ionization （ESI+） mode, quasi-molecular ion in the first order mass spectrometry of the unknown compound was 195.092 6 and its molecular formula was inferred to be C10H11FN2O. The fragment ions in the mass spectrometry of the unknown compound were compared with the related fragment ions of 4,4'-dimethylaminorex （4,4'-DMAR） in literature. It was found that the main fragment ions of the unknown compound were all 4 bigger than the corresponding fragment ions of 4,4'-DMAR. Therefore, the unknown compound was inferred to be a 4,4'-DMAR analogue with a methyl substituted by a fluorine in the benzene ring. The equivalent protons at δ=7.30 and δ=7.06 in 1H-nuclear magnetic resonance （1H-NMR） spectra and the characteristic spin-spin coupling constants （1JC-F=245.2 Hz, 2JC-F=21.3 Hz, 3JC-F=8.1 Hz） for 13C-19F interactions in carbon spectra, further proved that the fluorine substituted methyl at the para-position of the benzene ring. Finally, the unknown compound was determined as 4'-F-4-MAR. Conclusion A method that comprehensively used the identification materials 4'-F-4-MAR in GC-MS, UPLC-QTOF-MS, NMR and FTIR is established and the fragmentation mechanism of fragmentation ions of 4'-F-4-MAR created under the two modes -- electron impact （EI） and electrospray ionization under collision induced dissociation （ESI-CID） is deduced. The information will assist forensic science laboratories in identifying this compound or other substances with similar structure in their case work.

Relationship between Postmortem Interval and FTIR Spectroscopy Changes of the Rat Skin.

ABSTRACT: Objective To infer postmortem interval （PMI） based on spectral changes of the dorsal skin of rats within 15 days postmortem using Fourier transform infrared （FTIR） spectroscopy. Methods The rats were sacrificed by cervical dislocation after anesthesia, and then placed at 25 ℃ and relative humidity of 50%. The FTIR spectral data collected from the dorsal skin at PMI points were modeled with machine learning technique. Results There was no significant difference of absorption peak location among all the PMI groups but their peak intensities changed as a function of PMIs. The model for PMI estimation was constructed using partial least squares （PLS） regression, reaching a R2 of 0.92 and a root mean square error （RMSE） of 1.30 d. As shown in variable importance for projection （VIP）, four spectral bands including 1 760-1 700 cm-1, 1 660-1 640 cm-1, 1 580-1 540 cm-1 and 1 460-1 420 cm-1 were determined as important contributions to model prediction. Conclusion Application of the FTIR technique to detect postmortem spectral changes of the rat skin provides a novel proposal for PMI estimation.

Determination of Electrocution Using Fourier Transform Infrared Microspectroscopy and Machine Learning Algorithm.

ABSTRACT: Objective To analyze the differences among electrical damage, burns and abrasions in pig skin using Fourier transform infrared microspectroscopy （FTIR-MSP） combined with machine learning algorithm, to construct three kinds of skin injury determination models and select characteristic markers of electric injuries, in order to provide a new method for skin electric mark identification. Methods Models of electrical damage, burns and abrasions in pig skin were established. Morphological changes of different injuries were examined using traditional HE staining. The FTIR-MSP was used to detect the epidermal cell spectrum. Principal component method and partial least squares method were used to analyze the injury classification. Linear discriminant and support vector machine were used to construct the classification model, and factor loading was used to select the characteristic markers. Results Compared with the control group, the epidermal cells of the electrical damage group, burn group and abrasion group showed polarization, which was more obvious in the electrical damage group and burn group. Different types of damage was distinguished by principal component and partial least squares method. Linear discriminant and support vector machine models could effectively diagnose different damages. The absorption peaks at 2 923 cm-1, 2 854 cm-1, 1 623 cm-1, and 1 535 cm-1 showed significant differences in different injury groups. The peak intensity of electrical injury's 2 923 cm-1 absorption peak was the highest. Conclusion FTIR-MSP combined with machine learning algorithm provides a new technique to diagnose skin electrical damage and identification electrocution.

Structure Analysis and Characterization of Aminorex Analogue 4'-F-4-MAR / 法医学杂志

Objective To study the identification method for 4'-F-4-methylaminorex （4'-F-4-MAR） in samples without reference substance. Methods Gas chromatography-mass spectrometry （GC-MS）, ultra-high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry （UPLC-QTOF-MS）, nuclear magnetic resonance （NMR） and Fourier transform infrared （FTIR） were comprehensively used for the structure identification of 4'-F-4-MAR in samples. Results Under the positive electrospray ionization （ESI+） mode, quasi-molecular ion in the first order mass spectrometry of the unknown compound was 195.092 6 and its molecular formula was inferred to be C10H11FN2O. The fragment ions in the mass spectrometry of the unknown compound were compared with the related fragment ions of 4,4'-dimethylaminorex （4,4'-DMAR） in literature. It was found that the main fragment ions of the unknown compound were all 4 bigger than the corresponding fragment ions of 4,4'-DMAR. Therefore, the unknown compound was inferred to be a 4,4'-DMAR analogue with a methyl substituted by a fluorine in the benzene ring. The equivalent protons at δ=7.30 and δ=7.06 in 1H-nuclear magnetic resonance （1H-NMR） spectra and the characteristic spin-spin coupling constants （1JC-F=245.2 Hz, 2JC-F=21.3 Hz, 3JC-F=8.1 Hz） for 13C-19F interactions in carbon spectra, further proved that the fluorine substituted methyl at the para-position of the benzene ring. Finally, the unknown compound was determined as 4'-F-4-MAR. Conclusion A method that comprehensively used the identification materials 4'-F-4-MAR in GC-MS, UPLC-QTOF-MS, NMR and FTIR is established and the fragmentation mechanism of fragmentation ions of 4'-F-4-MAR created under the two modes -- electron impact （EI） and electrospray ionization under collision induced dissociation （ESI-CID） is deduced. The information will assist forensic science laboratories in identifying this compound or other substances with similar structure in their case work.

Relationship between Postmortem Interval and FTIR Spectroscopy Changes of the Rat Skin / 法医学杂志

Objective To infer postmortem interval （PMI） based on spectral changes of the dorsal skin of rats within 15 days postmortem using Fourier transform infrared （FTIR） spectroscopy. Methods The rats were sacrificed by cervical dislocation after anesthesia, and then placed at 25 ℃ and relative humidity of 50%. The FTIR spectral data collected from the dorsal skin at PMI points were modeled with machine learning technique. Results There was no significant difference of absorption peak location among all the PMI groups but their peak intensities changed as a function of PMIs. The model for PMI estimation was constructed using partial least squares （PLS） regression, reaching a R2 of 0.92 and a root mean square error （RMSE） of 1.30 d. As shown in variable importance for projection （VIP）, four spectral bands including 1 760-1 700 cm-1, 1 660-1 640 cm-1, 1 580-1 540 cm-1 and 1 460-1 420 cm-1 were determined as important contributions to model prediction. Conclusion Application of the FTIR technique to detect postmortem spectral changes of the rat skin provides a novel proposal for PMI estimation.

Determination of Electrocution Using Fourier Transform Infrared Microspectroscopy and Machine Learning Algorithm / 法医学杂志

Objective To analyze the differences among electrical damage, burns and abrasions in pig skin using Fourier transform infrared microspectroscopy （FTIR-MSP） combined with machine learning algorithm, to construct three kinds of skin injury determination models and select characteristic markers of electric injuries, in order to provide a new method for skin electric mark identification. Methods Models of electrical damage, burns and abrasions in pig skin were established. Morphological changes of different injuries were examined using traditional HE staining. The FTIR-MSP was used to detect the epidermal cell spectrum. Principal component method and partial least squares method were used to analyze the injury classification. Linear discriminant and support vector machine were used to construct the classification model, and factor loading was used to select the characteristic markers. Results Compared with the control group, the epidermal cells of the electrical damage group, burn group and abrasion group showed polarization, which was more obvious in the electrical damage group and burn group. Different types of damage was distinguished by principal component and partial least squares method. Linear discriminant and support vector machine models could effectively diagnose different damages. The absorption peaks at 2 923 cm-1, 2 854 cm-1, 1 623 cm-1, and 1 535 cm-1 showed significant differences in different injury groups. The peak intensity of electrical injury's 2 923 cm-1 absorption peak was the highest. Conclusion FTIR-MSP combined with machine learning algorithm provides a new technique to diagnose skin electrical damage and identification electrocution.

Correlation between mechanical properties and stabilization time of chemical bonds in glass-ionomer cements

Abstract The objective was to evaluate the compressive strength (CS), diametral tensile strength (DTS), flexural strength (FS), and Knoop microhardness (KH) of different conventional restorative glass-ionomer cements (GICs) and to correlate these mechanical properties (MP) with the stabilization time (ST) of their chemical bonds. Eighteen GICs were tested: Bioglass [B], Chemfil Rock [CR], Equia Forte [EF], Gold Label 2 [GL2], Gold Label 9 [GL9], Glass Ionomer Cement II [GI], Ionglass [IG], Ion Z[ IZ], Ionomaster [IM], Ionofil Plus [IP], Ionostar Plus [IS], Ketac Molar Easymix [KM], Magic Glass [MG], Maxxion R [Ma], Riva Self Cure [R], Vidrion R [V], Vitro Fil [VF] and Vitro Molar [VM]. The mechanical strength tests were performed in a universal testing machine. KH readings were done with a diamond indenter. STs were examined by Fourier Transform Infrared spectroscopy (FTIR). Data were analyzed with ANOVA and Tukey test (p<0.05). The Spearman rank test was used to evaluate the dependence between the MPs and ST results. The highest MP values were EF, GL2, GL9, GI and KM and the lowest for MG, MA, B, VF and IM. The longest ST was for GL2 and the shortest was for B. ST correlated positively with MP. GICs with longer chemical bonds ST are generally stronger and the ST value obtained from FTIR was useful in predicting the strength of GICs tested.

Bond stability of universal adhesives applied to dentin using etch-and-rinse or self-etch strategies

Abstract This study evaluated the immediate and 6-month dentin bond strength of universal adhesives used in etch-and-rinse or self-etch bonding strategies. The adhesives tested were Ambar Universal, G-Bond, Single Bond Universal, Tetric N-Bond Universal, and Ybond Universal. Gold standard adhesives (Scotchbond Multipurpose Plus and Clearfil SE Bond) were controls. Microtensile dentin bond strength (n=5 teeth), pH, and C=C conversion (n=3) were evaluated. Data were analyzed at α=0.05. All adhesives showed differences in pH. Ybond had intermediately strong aggressiveness, whereas the others were ultra-mild. The C=C conversion was different in most adhesives. In the etch-and-rinse strategy, all adhesives showed similar results generally except for G-Bond, which had lower bond strength than most adhesives. G-Bond and Tetric-N-Bond showed lower bond strengths after 6 months compared with 24 h, whereas the other adhesives had stable dentin bonds. In the self-etch strategy, G-Bond had lower bond strength than most adhesives. After 6 months, Ambar was the only adhesive showing lower dentin bond strength compared with 24 h. Most adhesives had discreet drops in bond strength during aging when used in the self-etch strategy. The failure modes were also material dependent, with a general pattern of increased adhesive and/or pre-testing failures after storage. In conclusion, the bonding performance of universal adhesives to dentin is material dependent. Most adhesives had stable dentin bonds with results comparable to the gold standard materials, particularly when applied in the self-etch mode. In general, it seems the use of universal adhesives in dentin should not be preceded by phosphoric acid etching.

Resumo Este estudo avaliou a resistência de união à dentina imediata e após 6 meses de adesivos universais utilizando estratégias de união convencional ou autocondicionante. Os adesivos testados foram Ambar Universal, G-Bond, Single Bond Universal, Tetric N-Bond Universal e Ybond Universal. Adesivos padrão-ouro (Scotchbond Multipurpose Plus e Clearfil SE Bond) foram os controles. Resistência de união à microtração na dentina (n=5 dentes), pH e conversão de C=C (n=3) foram avaliados. Os dados foram analisados considerando α=0,05. Todos os adesivos mostraram diferenças de pH comparados aos demais. Ybond Universal teve agressividade intermediária forte, enquanto os outros foram ultramoderados. A conversão de C=C foi diferente em quase todos adesivos. No modo convencional, em geral todos os adesivos mostraram resultados similares exceto G-Bond, que teve menor resistência de união que a maioria dos adesivos. G-Bond e Tetric-N-Bond mostraram resistências de união menores após 6 meses comparados a 24 h, enquanto os outros adesivos apresentaram estável união à dentina. No modo autocondicionante, G-Bond teve menor resistência de união que quase todos os adesivos. Após 6 meses, Ambar foi o único adesivo mostrando menor resistência de união à dentina comparado a 24 h. A maioria dos adesivos teve discreta queda na resistência de união durante o envelhecimento quando usados na estratégia autocondicionante. Os modos de falha também foram material dependentes, com um padrão geral de mais falhas adesivas e/ou pré-teste após o armazenamento. Em conclusão, o desempenho de união de adesivos universais à dentina é material dependente. Grande parte dos adesivos apresentou estável união à dentina com resultados comparáveis ao materiais padrão-ouro, particularmente quando aplicados no modo autocondicionante. Em geral, parece que o uso de adesivos universais em dentina não deve ser precedido por condicionamento com ácido fosfórico.

Simulated biological fluid exposure changes nanoceria's surface properties but not its biological response.

Nanoscale cerium dioxide (nanoceria) has industrial applications, capitalizing on its catalytic, abrasive, and energy storage properties. It auto-catalytically cycles between Ce3+ and Ce4+, giving it pro-and anti-oxidative properties. The latter mediates beneficial effects in models of diseases that have oxidative stress/inflammation components. Engineered nanoparticles become coated after body fluid exposure, creating a corona, which can greatly influence their fate and effects. Very little has been reported about nanoceria surface changes and biological effects after pulmonary or gastrointestinal fluid exposure. The study objective was to address the hypothesis that simulated biological fluid (SBF) exposure changes nanoceria's surface properties and biological activity. This was investigated by measuring the physicochemical properties of nanoceria with a citric acid coating (size; morphology; crystal structure; surface elemental composition, charge, and functional groups; and weight) before and after exposure to simulated lung, gastric, and intestinal fluids. SBF-exposed nanoceria biological effect was assessed as A549 or Caco-2 cell resazurin metabolism and mitochondrial oxygen consumption rate. SBF exposure resulted in loss or overcoating of nanoceria's surface citrate, greater nanoceria agglomeration, deposition of some SBF components on nanoceria's surface, and small changes in its zeta potential. The engineered nanoceria and SBF-exposed nanoceria produced no statistically significant changes in cell viability or cellular oxygen consumption rates.

Biodecolorization and Biodegradation of Azo Dye Reactive Orange-16 by Marine Nocardiopsis sp.

BACKGROUND: Azo dyes are xenobiotic compounds that have bioaccumulated in the environment due to escalated industrial development. These are hazardous in nature, possessing carcinogenic and mutagenic effects on human beings. OBJECTIVES: The perspective of the present study was to isolate and to determine azo dye (Reactive Orange-16) degrading potential of marine actinobacteria isolated from sediment samples of Port Blair, India. MATERIAL AND METHODS: Actinobacteria with dye decolorization potential were isolated from sea sediment samples. The actinobacterial isolate with the highest dye decolorizing percentage was identified with the help of phenotypic, biochemical and molecular studies. The different physico-chemical parameters for dye decolorization were also optimized. The nature of decolorization by the potent isolate was determined with the help of High Performance Liquid chromatography (HPLC) and Fourier Transformed Infrared spectroscopy (FTIR) techniques. Further the toxicity of RO-16 decolorized products was investigated with the help of phytotoxcity assay. RESULTS: Out of six actinobacterial isolates, VITVAMB 1 possessed the most efficient RO-16 decolorization property. It decolorized 85.6% of RO-16 (250 mg L-1) within 24hrs. Isolate VITVAMB 1 was identified to be Nocardiopsis sp. Maximum dye decolorization occurred at pH 8, temperature 35°C, 3% salt concentration and a dye concentration of 50 mg L-1. CONCLUSIONS: The nature of decolorization by Nocardiopsis sp. was biodegradation. Additionally, the degraded dye metabolites were found to be less toxic than pure dye. The high decolorization potential of VITVAMB 1 and the low toxicity of its degradation products make it a prospective dye removal system. The marine origin of VITVAMB 1 also makes it an attractive source for novel azo dye reducing enzymes.

[Effects of Temperature on FTIR Spectral Characteristics of Renal Tissue in Rats after Death].

OBJECTIVES: To analyse the Fourier transform infrared （FTIR） spectral data of renal tissue at different temperatures in rats after death, and to explore the effects of temperature on the FTIR spectral characteristics of renal tissue. METHODS: The rats were sacrificed by cervical dislocation and placed at 4 ℃, 20 ℃ and 30 ℃. The FTIR spectral data of renal tissue were collected at different time points and analysed by data mining method. RESULTS: The principal component analysis （PCA） results showed that there were significant trends of clustering in the samples of partial time point at 4 ℃, 20 ℃ and 30 ℃. Partial least square （PLS） regression models were established with the spectral data at three temperature groups. The performance of PLS regression models in 20 ℃ and 30 ℃ groups were more superior than that in 4 ℃ group, and the stability of the model in 20 ℃ group was better than that in 30 ℃ group. CONCLUSIONS: There are differences in the FTIR spectral characteristics of renal tissue of rats after death at different temperatures. Temperature has a major impact on the performance of FTIR spectral PLS regression model. Therefore, in order to improve the accuracy of postmortem interval estimation, the effects of temperature on the model should be considered in the related study by spectral method.

[Establishment of the Mathematical Model for PMI Estimation Using FTIR Spectroscopy and Data Mining Method].

OBJECTIVES: To analyse the relationship between Fourier transform infrared （FTIR） spectrum of rat's spleen tissue and postmortem interval （PMI） for PMI estimation using FTIR spectroscopy combined with data mining method. METHODS: Rats were sacrificed by cervical dislocation, and the cadavers were placed at 20 ℃. The FTIR spectrum data of rats' spleen tissues were taken and measured at different time points. After pretreatment, the data was analysed by data mining method. RESULTS: The absorption peak intensity of rat's spleen tissue spectrum changed with the PMI, while the absorption peak position was unchanged. The results of principal component analysis （PCA） showed that the cumulative contribution rate of the first three principal components was 96%. There was an obvious clustering tendency for the spectrum sample at each time point. The methods of partial least squares discriminant analysis （PLS-DA） and support vector machine classification （SVMC） effectively divided the spectrum samples with different PMI into four categories （0-24 h, 48-72 h, 96-120 h and 144-168 h）. The determination coefficient （R²ï¼‰ of the PMI estimation model established by PLS regression analysis was 0.96, and the root mean square error of calibration （RMSEC） and root mean square error of cross validation （RMSECV） were 9.90 h and 11.39 h respectively. In prediction set, the R² was 0.97, and the root mean square error of prediction （RMSEP） was 10.49 h. CONCLUSIONS: The FTIR spectrum of the rat's spleen tissue can be effectively analyzed qualitatively and quantitatively by the combination of FTIR spectroscopy and data mining method, and the classification and PLS regression models can be established for PMI estimation.

Infrared Spectral Characteristics of Electrical Injuries on Swine Skin Caused by Different Voltages Based on Machine Learning Algorithms.

OBJECTIVES: To explore infrared spectrum characteristics of different voltages induced electrical injuries on swine skin by using Fourier transform infrared-microspectroscopy （FTIR-MSP） combined with machine learning algorithms, thus to provide a reference to the identification of electrical skin injuries caused by different voltages. METHODS: Electrical skin injury model was established on swines. The skin was exposed to 110 V, 220 V and 380 V electric shock for 30 s and then samples were took, with normal skin tissues around the injuries as the control. Combined with the results of continuous section HE staining, the FTIR-MSP spectral data of the corresponding skin tissues were acquired. With the combination of machine learning algorithms such as principal component analysis （PCA） and partial least squares-discriminant analysis （PLS-DA）, different spectral bands were selected （full band 4 000-1 000 cm-1 and sub-bands 4 000-3 600 cm-1, 3 600-2 800 cm-1, 2 800-1 800 cm-1, and 1 800-1 000 cm-1）, and various pretreatment methods were used such as orthogonal signal correction （OSC）, standard normal variables （SNV）, multivariate scatter correction （MSC）, normalization, and smoothing. Thus, the model was optimized, and the classification effects were compared. RESULTS: Compared with simple spectrum analysis, PCA seemed to be better at distinguishing electrical shock groups from the control, but was not able to distinguish different voltages induced groups. PLS-DA based on the 3 600-2 800 cm-1 band was used to identify the different voltages induced skin injuries. The OSC could further optimize the robustness of the 3 600-2 800 cm-1 band model. CONCLUSIONS: It is feasible to identify electrical skin injuries caused by different voltages by using FTIR-MSP technique along with machine learning algorithms.

Effects of Temperature on FTIR Spectral Characteristics of Renal Tissue in Rats after Death / 法医学杂志

OBJECTIVES@#To analyse the Fourier transform infrared （FTIR） spectral data of renal tissue at different temperatures in rats after death, and to explore the effects of temperature on the FTIR spectral characteristics of renal tissue.@*METHODS@#The rats were sacrificed by cervical dislocation and placed at 4 ℃, 20 ℃ and 30 ℃. The FTIR spectral data of renal tissue were collected at different time points and analysed by data mining method.@*RESULTS@#The principal component analysis （PCA） results showed that there were significant trends of clustering in the samples of partial time point at 4 ℃, 20 ℃ and 30 ℃. Partial least square （PLS） regression models were established with the spectral data at three temperature groups. The performance of PLS regression models in 20 ℃ and 30 ℃ groups were more superior than that in 4 ℃ group, and the stability of the model in 20 ℃ group was better than that in 30 ℃ group.@*CONCLUSIONS@#There are differences in the FTIR spectral characteristics of renal tissue of rats after death at different temperatures. Temperature has a major impact on the performance of FTIR spectral PLS regression model. Therefore, in order to improve the accuracy of postmortem interval estimation, the effects of temperature on the model should be considered in the related study by spectral method.