Real time estimation of CO2 laser weld quality for automotive industry

Laser welding is one of the most precise welding processes in joining sheet metals. In laser welding, performing real time evaluation of the welding quality is very important to enhance the efficiency of the welding process. In this study, the plasma and spatter, which are generated during laser welding, are measured using UV and IR photodiodes. The factors that influence weld quality are classified into five categories; optimal heat input, slightly low heat input, low heat input, partial joining due to gap mismatch, and nozzle deviation. The data number deviated from reference signals and their standard deviations were also considered to evaluate the qualities. A system was also formulated to perform real time evaluations of the weld quality using a fuzzy multi-feature pattern recognition with the measured signals.     

Efficiency of four different techniques in coupled HPLC-UV/VIS to quantify overlapping peaks with known spectral features

Summary Four different techniques to quantify unresolved chromatographic peaks with known spectral features combined with photodiode array detection, are investigated as regards their efficiency for the accurate and precise determination of drugs in the low g-range. The comparison includes peak suppression utilising difference chromatograms, first-order derivative chromatograms, selective chromatograms, generated by the calculation of orthogonal polynomial shares, and the powerful least-squares multicomponent analysis approach. Each of these methods uses UV-spectra taken throughout, the peak. The results presented and conclusions reached should enable the chromatographer to come to a decision about the reasonable use of these options now provided by multichannel detection in HPLC.     

Simplified Solid-Phase Extraction Procedure and Liquid Chromatographic Determination of Celecoxib in Rat Serum

A simplified solid phase extraction method, eliminating a preliminary protein precipitation has been developed for the determination of celecoxib in rat plasma. The technique included a solid phase extraction of the serum samples on a [poly (divinylbenzene-co-N-vinylpyrrolidone)] sorbent. After conditioning, the cartridge was loaded with 0.5 mL of acidified serum containing internal standard. Elution was made with 1 mL of a mixture of acetonitrile and methanol (1/1, v/v). After evaporation of the eluate to dryness and reconstitution with methanol, the samples were analyzed on an octadecyl bonded phase with several mobile phases containing acetonitrile and a phosphate buffer. Detection was carried out using a Photodiode Array Detector. Full validation of the proposed method was provided (linearity range: 0.01–2 mg. L^–1, average extraction efficiency: 92.4%; average intra-day variability: 4.6% with an accuracy of 94.8%; average interday variability: 5% with an accuracy of 95.3%, limit of detection: 0.005 mg. L^–1, limit of quantification: 0.002 mg. L^–1). The proposed method was successfully utilised to quantify celecoxib in rat plasma for a pharmacokinetic study.Revised: 26 January and 23 April 2004     

Effect of drying temperature and blanching on the degradation of chlorophyll a and b in mint (Mentha spicata Huds.) and basil (Ocimum basilicum): Analysis by high performance liquid chromatography with photodiode array detection

Summary The effect of drying conditions on the preservation of chlorophyll pigments in mint and basil have been investigated in order to determine the effects of drying temperature and whether or not there was a prior blanching.Pigments extracted from fresh and dried samples were analyzed by reversed phase high performance liquid chromatography coupled to a photodiode array detector; isocratic separation was performed on a Zorbax ODS C18 column.The purity of the chromatographic peaks of chlorophylls and breakdown products was investigated. The visible spectra of standard samples of chlorophylls and pheophytins were compared, using least squares normalization with those of peaks from the extracts of fresh and dried mint and basil. The study has shown that chlorophylls were better preserved when drying was preceded by a short blanching; if samples were not blanched before drying, the degradation of chlorophylls a and b was best prevented by drying at low temperatures.     

PAD在HPLC分析长春胺中的应用

本文报道用光电二极管阵列检测器(PAD)鉴定小蔓和大蔓长春花中的长春胺。并对经典制备方法得到的长春胺样品进行了纯度判断。利用建立的紫外光谱数据库对长春胺中的分解产物进行光谱检索和鉴定。测定了长春胺的稳定性。     

利用凝胶渗透色谱示差-紫外检测器联用测定丁苯共聚物的组成分布

将凝胶渗透色谱(GPC)中的示差与紫外检测器联用,测定了无规共聚丁苯橡胶和SBS三元嵌段共聚物中各级分的组成变化.实验方法选择中对比了两种浓度参数的确定方法,发现通过改变注射量来实现浓度变化的方法优于使用系列浓度样品的方法.分别测定标准样品在紫外和示差检测器上信号产生的时间间隔可以确定两个检测器上信号的时间差.根据紫外-示差检测器联用可以看到SBR无规共聚物和三嵌段SBS共聚物样品中每一个级分中随着相对分子质量的变化,苯乙烯含量的变化.     

Sensitive analyses of agricultural chemicals by capillary electrochromatography

Capillary electrochromatography using a monolithic matrix was employed to develop a rapid and highly efficient separation methodology for the analyses of mixtures of agrochemical importance. Using this method, ppm‐ppb detection limits for urea, carbamate, and phenoxy acid herbicides were achieved without a preconcentration technique. The detection limits were further decreased to low‐ppb levels for the same class of compounds using an on‐column preconcentration technique.     

Rapid separation of four main taxoids in Taxus species by a combined LLP-SPE-HPLC (PAD) procedure

A method is described for the simultaneous determination of paclitaxel and three related taxoids, 10-deacetylbaccatin III (10-DAB III), baccatin III, and cephalomannine, in the extracts from the needles of three Chinese yew species, Taxus cuspidata, T. chinensis, and T. media. SPE was applied as the sample preparation technique and RP-HPLC with a photodiode array detector (PAD) was used for the analysis of extract samples. The crude extracts were treated with an improved SPE cartridge packed with a combination of 1-vinyl-pyrrolidin-2-one and divinyl-benzene. The eluent was 75% methanol. The following separation was achieved with a gradient program on an HIQ SIL C18W column in a system of ACN/water within 60 min. The samples were detected by PAD at wavelengths of 232.1 nm for 10-DAB III, 229.8 nm for baccatin III and paclitaxel, and 223.9 nm for cephalomannine. The content of 10-DAB III, baccatin III, cephalomannine, and paclitaxel varied from 0.0277 to 0.0875, 0.0254 to 0.0405, 0.0715 to 0.2486, and 0.0996 to 0.1301 mg/g in fresh needles of the above yew species, respectively. The assay achieved good resolution in the separation between the four compounds, and it can be used for quality control or purity determination for those in bulk and pharmceutical dosage forms.     

Chemical screening of olive biophenol extracts by hyphenated liquid chromatography

Chemical screening using reversed phase HPLC-photodiode array detection (RPLC-DAD) and RPLC-electrospray ionisation mass spectrometry (RPLC-ESI-MS) is widely applied as an approach to streamline natural products research. The full potential of this approach is demonstrated in this paper by application to the chemical screening of olive products including olive mill waste (OMW). Out of 100 biophenols previously reported in olive products, the on-line RPLC-DAD-ESI-MS was able to confirm the presence of 52 compounds in OMW. This included a number of simple phenols, flavonoids and secoiridoids. By careful examination of the combined DAD and ESI-MS data, extra information was elucidated including: the site of glycosidation on the phenol ring of hydroxytyrosol; the identity of the other luteolin-glucoside isomer as luteolin-4′-O-glucoside; identifying rutin rather than the previously reported hesperidin (and the reasons for possible mis-assignment); and the detection of diastereomers of 4-hydroxyphenylethyl alcohol-deacetoxy elenolic acid dialdehyde (4-HPEA-DEDA) and 3,4-dihydroxyphenylethyl alcohol-deacetoxy elenolic acid dialdehyde (3,4-DHPEA-DEDA).     

凤凰木种子毒蛋白的高效凝胶过滤色谱分析

介绍用ＨＰＧＦＣ（高效凝胶过滤色谱）对凤凰木种子中提取的３种毒蛋白分别进行色谱分析。并对分离的蛋白峰进行紫外光谱扫描来确认蛋白的纯度。根椐标准相对分子质量曲线,分别得到它们的相对分子质量并与ＳＤＳ－ＰＡＧＦ（十二烷基磺酸钠－聚丙烯酰胺凝胶电泳）所得结果进行比较,用柱后衍生法测定了３个蛋白各自的氨基酸组成。