基于K-S算法的水质硝酸盐含量光谱检测方法研究

应用紫外光谱对水体中的总氮进行测定,常规的测定方法在分析精度上依赖于所建立的光谱数学模型.测量过程中所依据的紫外光谱数据波段较多,模型的建立所依据的测试样本也比较多,因而很容易引入干扰光谱信息.对水质样本的原始光谱进行一阶微分处理后,采用Kennard-Stone算法对41个样本进行优选,选出30个作为训练集,剩余11...     

不同提取方法对小花棘豆总生物碱提取率的影响

采用乙醇浸提-有机溶剂萃取法、超声波辅助提取法、乙醇浸提-柱层析分离法3种方法提取小花棘豆中的总生物碱,比较3种方法总生物碱的提取率.3种方法的总生物碱提取率分别为0.0008％、0.0032％、0.0080％.故选用乙醇浸提-柱层析分离法.通过正交试验,得到乙醇浸提最佳工艺条件为:提取温度30℃,乙醇浓度75％,物料...     

碘回收工艺中硫酸盐含量的快速测定

介绍了一种用UV-1600型紫外可见分光光度计快速测定碘回收工艺中硫酸盐含量的方法.以氯化镁、乙酸钠、硝酸钾和乙醇为缓冲溶液,在440nm处测量吸光度,硫酸盐浓度在0-50μg/mL符合比耳定律,可决系数为0.9996.将所得碘吸收液中硫酸盐含量与重量法所得结果对比,确定分光光度法是实验室快速测定碘回收工艺中硫酸盐含量...     

荧光分析法在环境有机污染物检测中的应用

综述了近十年来荧光分析法在环境有机污染物检测中的应用,主要介绍了国内的应用情况.依据检测时所采用的方法如直接荧光分析法、间接荧光分析法及其他的一些荧光分析方法分别进行归纳总结.     

蔬菜中铁含量的测定及方法比较

用分光光度法直接测定蔬菜中铁的含量,方法简便、快速、准确.分别采用浓盐酸和浓硫酸两种消解方法对样品进行处理,并对其测定结果进行比较,实验结果表明,浓硫酸消解法消解能力更强,测定更为准确.5种蔬菜中木耳铁含量最高,对指导人们合理食用蔬菜进行补铁及进一步开发蔬菜产品提供了可靠的理论依据.     

Development and validation of a sequential-injection method with chemiluminescence detection for the high throughput assay of the total antioxidant capacity of wines

This work reports a sequential-injection analysis (SIA) method with chemiluminescence (CL) detection for the rapid assay of the total antioxidant capacity (TAC) in wines. The method exploited the Co(II)-catalysed CL reaction of luminol with hydrogen peroxide in alkaline medium. Zones of sample, hydrogen peroxide, catalyst (Co(II) solution) and alkaline luminol were sequentially aspirated into the holding coil of the SIA manifold. Then, the flow was reversed and the stacked zones were directed to the CL detector. As the zones overlapped, antioxidants in the samples scavenged a portion of hydrogen peroxide and the decrease in the CL intensity was monitored and related to the TAC. The chemical and geometric conditions were studied and the method was validated in terms of linearity, accuracy (trueness and precision), matrix effects, signal additivity and robustness. The reproducibility of the method (expressed as the between-days % relative standard deviation) was between 2.5 and 3.4% and the trueness (expressed as the % recovery in wines spiked with gallic acid) was in the range 96.7-97.3%. The sampling frequency was 60 samples h⁻¹. The proposed SIA-CL method was compared with the DPPH method and the Folin-Ciocalteau (FC) method for the analysis of 25 wine samples.     

数据统计处理中关于相关系数R的错误理解

本文旨在纠正一种在化学家中流传甚久的对统计数学中相关系数的错误理解.这种理解认为在数据拟合中单凭相关系数R大于某个人为指定值就可以判定数据拟合的优劣.     

连续激光干扰效果评估方法北大核心CSCD

采用改进后的图像相关度计算方法,在精确配准干扰前后图像的基础上,以像素为单位计算图像相关度,根据人眼识别效果在评估前确定干扰阈值,计算图像有效干扰像元统计值,定量描述激光干扰效果;开展多波段激光干扰成像系统试验,采集不同干扰功率下的激光干扰图像,评估干扰效果。结果表明,该方法能精确识别图像局部变化,客观反映图像质量变化,对各波段不同功率下的激光干扰成像图像给出科学评估结果,对单对图像的处理速度优于s级,具有一定的工程应用价值。     

Development and Validation of Stability-Indicating HPLC Methods for Quantitative Determination of Pravastatin,Fluvastatin, Atorvastatin,and Rosuvastatin in Pharmaceuticals

Abstract

High-performance liquid-chromatographic (HPLC) methods were validated for determination of pravastatin sodium (PS), fluvastatin sodium (FVS), atorvastatin calcium (ATC), and rosuvastatin calcium (RC) in pharmaceuticals. Two stability-indicating HPLC methods were developed with a small change (10%) in the composition of the organic modifier in the mobile phase. The HPLC method for each statin was validated using isocratic elution. An RP-18 column was used with mobile phases consisting of methanol–water (60:40, v/v, for PS and RC and 70:30, v/v, for FVS and ATC). The pH of each mobile phase was adjusted to 3.0 with orthophosphoric acid, and the flow rate was 1.0 mL/min. Calibration plots showed correlation coefficients (r) > 0.999, which were calculated by the least square method. The detection limit (DL) and quantitation limit (QL) were 1.22 and 3.08 µg/mL for PS, 2.02 and 6.12 µg/mL for FVS, 0.44 and 1.34 µg/mL for ATC, and 1.55 and 4.70 µg/mL for RC. Intraday and interday relative standard deviations (RSDs) were <2.0%. The methods were applied successfully for quantitative determination of statins in pharmaceuticals.     

Simultaneous Extraction and Atomic Absorption Spectrometric Determination of IB Group Elements (Cu,Ag, Au) from Aqueous Thiocyanate/2,2′-Dipyridyl-2-Pyridylhydrazone (Dpph) Solutions

Abstract

A quantitative simultaneous extraction procedure of copper, silver and gold cations from aqueous thiocyanate solutions into Methyl Isobutyl Ketone (MIBK) is described. the effects of pH, thiocyanate and 2,2′-Dipyridyl-2-py-ridylhydrazone (DPPH) concentration were studied. Tolerance amounts for many diverse cations and anions have been determined. Finally, a procedure for the determination of IB Group elements is recommended, by extaction-AAS.