原子吸收光谱法测定磷酸酯化梨渣吸附的Cr（Ⅵ）离子

通过原子吸收光谱法研究了在不同pH值、吸附剂量、吸附质浓度和吸附时间条件下磷酸酯化改性梨渣吸附Cr（Ⅵ）离子的效果。溶液初始pH 4.5时,Cr（Ⅵ）离子的吸附达到最大值;酯化梨渣≥10g.L-1能除去Cr（Ⅵ）为100μg.L-1溶液中的86.5%的Cr（Ⅵ）离子。酯化梨渣对Cr（Ⅵ）离子的吸附符合Langmuir等温模型,其最大吸附能力为67.56μg.g-1。Cr（Ⅵ）离子达到吸附平衡的时间为90min,准一级反应动力学方程可描述酯化梨渣对Cr（Ⅵ）离子的吸附过程。     

Graphene grafted silica‐coated Fe3O4 nanocomposite as absorbent for enrichment of carbamates from cucumbers and pears prior to HPLC

In this paper, a novel graphene (G) grafted silica‐coated Fe₃O₄ nanocomposite was fabricated by the chemical bonding of G onto the surface of silica‐coated Fe₃O₄ nanoparticles. Some carbamates (metolcarb, carbaryl, pirimicarb, and diethofencarb) in cucumber and pear samples were enriched by this nanocomposite prior to their determination by HPLC with UV detection. Experimental parameters that may affect the extraction efficiency were investigated. Under the optimum conditions, a linear response was achieved in the concentration range of 0.5–100.0 ng/g for metolcarb, carbaryl, and diethofencarb, and 1.0–100 ng/g for pirimicarb with the correlation coefficients (r) ranging from 0.9956 to 0.9984. The LOD (S/N = 3) of the method were found to be in the range from 0.08 to 0.2 ng/g. The RSDs were in the range from 2.4 to 5.8%. The results indicated that the G grafted silica‐coated Fe₃O₄ nanocomposite was stable and efficient for magnetic SPE and has a great application potential for the preconcentration of other organic pollutants from real samples.     

杀菌剂抑霉唑在梨子中残留动态分析

提出了通过液-液萃取,而后用气相色谱方法测定梨中抑霉唑残留量的方法.对已报道的样品提取、纯化方法进行了改进.本试验以丙酮作提取剂,经乙酸乙酯萃取,用高灵敏度气相色谱μ-ECD检测器测定.方法检出限为0.01 mg/kg,平均回收率为80.5%～111.8%,相对标准偏差为0.3%～3.3%.该法可用于梨肉和梨皮中抑霉唑残留量的测定.同时,还对抑霉唑由梨皮向梨肉的迁移,在梨体上的降解等动态进行了测定.     

Prediction of soluble solids content, firmness and pH of pear by signals of electronic nose sensors

The objective of this study was to investigate the predictability of an electronic nose for fruit quality indices. Responses signal of sensor array in electronic nose were employed to establish quality indices model for “xueqing” pear. The relationships were established between signal of electronic nose and the quality indices of fruit (firmness, soluble solids content (SSC) and pH) by multiple linear regressions (MLR) and artificial neural network (ANN). The prediction models for firmness and soluble solids content indicated a good prediction performance. The SSC model by ANN had a standard error of prediction (SEP) of 0.41 and correlation coefficient 0.93 between predicted and measured values, the model by ANN for the penetrating force (CF) had a 3.12 SEP and 0.94 coefficient, respectively. The results imply that it is possible to predict “xueqing” pear quality characteristics from signal of E-nose.     

LS-SVM的梨可溶性固形物近红外光谱检测的特征波长筛选

为提高梨可溶性固形物含量(soluble solids content,SSC)的近红外光谱模型的精度和稳定性,以160个梨样品为实验对象,分别对原始光谱、多元散射校正(MSC)和标准正态变量变换(SNV)处理后的光谱,经无信息变量消除算法(UVE)挑选后,再结合遗传算法(GA)和连续投影算法(SPA),筛选梨可溶性固形物的近红外光谱特征波长。将筛选后的波长作为输入变量建立梨可溶性固形物的最小二乘支持向量机(LS-SVM)模型。结果表明经过SNV-UVE-GA-SPA从全波段3112个波长中筛选出的30个特征波长建立的梨可溶性固形物LS-SVM模型效果最好,该模型的预测集相关系数(R_p)和预测均方根误差(RMSEP)分别为0.956和0.271。该模型简单可靠,预测效果好,能满足梨的可溶性固形物含量的快速检测,为在线检测和便携式设备开发提供了理论基础。     

梨花粉红外波段复折射率测定与分析

花粉是生物气溶胶重要的组成部分,复折射率是研究花粉光学特性以及探测、识别生物气溶胶成分的重要参数。采用压片法对梨花粉2.5~15 μm波段的反射光谱进行了测量,利用Krames-Kronig(K-K)关系计算了复折射率,并就傅里叶红外光谱仪测试压片的入射角和复折射率长波长、短波长区外推两方面对结果作了误差分析。结果表明,测试时18°入射角以及长波长、短波长区外推对梨花粉复折射率的计算结果影响不大,利用反射光谱计算花粉复折射率的方法是可行的。计算得到的复折射率谱对梨花粉光学特性的研究以及生物气溶胶成分的探测、识别有一定的参考价值。     

水果坚实度的近红外光谱检测分析试验研究

应用傅里叶漫反射近红外光谱技术探讨了水果坚实度无损检测的方法。利用偏最小二乘法建立了坚实度与漫反射光谱的无损检测数学模型,同时对不同光谱预处理方法和不同建模波段范围对模型的预测性能进行了对比分析。结果表明：利用傅里叶变换光谱仪采集的原始光谱的平滑预处理对结果并没有太大影响;原始光谱在800～2 500 nm范围的模型得到了最好的预测结果：校正集样本的相关系数r为0.869,校正均方根误差RMSEC为3.88 N;预测集样本的相关系数r为0.840,预测均方根误差RMSEP为4.26 N。 通过本研究得出：应用近红外漫反射光谱检测水果坚实度是可行的,为今后快速无损评价水果成熟度提供了理论依据。     

Simultaneous determination of cypermethrin and permethrin in pear juice by ultrasound-assisted dispersive liquid-liquid microextraction combined with gas chromatography

A new method was developed for simultaneous determination of cypermethrin and permethrin residues in pear juice with ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and gas chromatography-flame ionization detection (GC-FID). 3.5 mL of methanol (dispersant) and 30 μL of C₂Cl₄ (extractant) were injected into 5.0 mL of pear juice sample and then emulsified by ultrasound for 2.0 min to forming the cloudy solution. Under the optimum condition, the enrichment factors for cypermethrin and permethrin were 344 and 351 fold respectively. Good linearity was observed in a range of 0.009-1.52 μg g⁻¹ with the correlation coefficient (r²)≥0.9993. The limits of detection (LODs) were 3.1 and 2.2 μg kg⁻¹ for cypermethrin and permethrin, respectively (S/N = 3). The recoveries of the method evaluated at three spiked levels were in the range of 92.1%-107.1%. The repeatability evaluated as intra-day and inter-day precision (RSDs) were less than 4.0% (n = 5). The developed method was successfully applied to determine the two pesticide residues in different pear juice samples.     

离子交换固相萃取-高效液相色谱法研究吡虫啉在梨中的分布及残留动态

建立一种以固相萃取(SPE)、高效液相色谱(HPLC)为基础的测定梨果皮、果肉中吡虫啉残留量的方法。样品用乙腈进行提取,经二氯甲烷液液分配后用阳离子交换固相萃取(SCX-SPE)柱净化,高效液相色谱/二极管阵列检测法(HPLC/DAD)测定。各种添加水平(果皮:0.05、0.1、0.5、2 mg/kg;果肉:0.05、0.5、1mg/kg)的回收率为83%~103%,相对标准偏差(RSD)小于10%,方法的检出限为0.05 mg/kg。运用此方法分别对梨果皮和果肉中吡虫啉的残留动态进行研究,发现吡虫啉主要在梨果皮中残留,得到吡虫啉在果皮中的消解动态方程为:wt=w0×exp(-0.235t),半衰期是2.98 d。     

基于Slope/Bias算法的相近种类水果模型传递研究

为了提升便携式近红外仪器中单一水果模型应用的广泛性,创新性的将不同仪器间模型传递的思想应用在不同种类水果间可溶性固形物(soluble solid content,SSC)的模型传递。基于苹果、梨、桃三种水果在SSC含量范围、果型大小以及果皮厚度等的相近物理化学特性,提出利用简单的斜率/截距(Slope/Bias)算法对苹果SSC的偏最小二乘(partial least square,PLS)模型进行传递,仅用少量的梨和桃样品即可将苹果SSC模型应用于其SSC值的预测,更快捷方便且节约成本。对于梨样品,用35个标准样品,预测集均方根误差(root mean square error of prediction,RMSEP)值由直接预测的1.009°Brix降为0.565°Brix;对于桃样品,用40个标准样品,RMSEP由直接预测的1.726°Brix降为0.677°Brix。为了验证该模型传递方法的可行性,通过斜率/截距算法,采用梨和桃模型对其他两种水果的SSC进行预测,其中利用建立的梨SSC模型,经斜率/截距算法模型传递后,对于苹果样品,用30个标准样品,RMSEP值达到0.597°Brix,对于桃样品,用40个标准样品,RMSEP值达到0.689°Brix;利用建立的桃SSC模型,经斜率/截距算法模型传递后,对于苹果样品,用35个标准样品,RMSEP值达到0.654°Brix,对于梨样品,用30个标准样品,RMSEP值达到0.439°Brix。研究结果表明:斜率/截距(Slope/Bias)方法可用于苹果、梨、桃等相近种类水果间的模型传递,为近红外光谱仪在相似种类物质间的预测提供了新思路。