非平衡体系中固相微萃取技术的定量分析研究——快速监测水中痕量的有机污染物(多环芳烃)

采用固相微萃取技术，以100μM膜厚的聚二甲基硅氧烷纤维萃取水中10种多环芳烃，在60MIn采样时间内纤维上的吸附量与采样的时间近乎成正比，分配体系达到平衡前可以定量地测定水中的待测物.该方法的线性范围在0.1~100μg/l，检出限在0.01~0.03μg/l，15μg/l的回收率在80%~100%，相对标准偏差在20%以

The preparation of SPME coating using manganese oxide nanorod and its applications in the analysis of acrylamide in food samples

采用水热法合成氧化锰纳米棒,并以物理涂渍的方法固定于不锈钢丝上,制备获得氧化锰纳米棒固相萃取(SPME)涂层.该涂层对丙烯酰胺具有较好的富集能力,且具有较强的机械强度.实验通过优化萃取时间、萃取温度、解吸温度、解吸时间以及离子强度等影响萃取效率的实验条件,建立了利用该SPME与气相色谱-电子捕获检测器分析法,进行了薯片和饼干中丙烯酰胺含量的检测.结果显示,氧化锰纳米棒纤维涂层对于上述两种具有复杂基质样品中的丙烯酰胺具有较好的萃取能力,实验测得的薯片和饼干中丙烯酰胺的含量分别为2.43和1.31 mg g~(-1).Novel manganese oxide nanorods were synthesized using hydro-thermal method and applied as a coating material for solid phase microextraction(SPME). The extraction efficiency of acrylamide using the coating was investigated. Extraction conditions including extraction time, extraction temperature, desorption temperature, desorption time and ionic strength in the SPME of acrylamide were optimized. Under the optimized conditions, the SPME-GC-ECD method was successfully applied in the determination of acrylamide in potato chip and cookies samples. The detection results reveal the excellent extraction ability towards acrylamide in the two complex matrix samples. The obtained contents of acrylamide for the selected samples were found to be 2.43 and 1.31 mg g~(-1).厦门市科技局高校创新项目(编号:3502Z20143025);; 福建省科技重大专项(编号:2011YZ0001-1)资助项

Application of Sol-gel Technology in Solid-phase Microextraction(SPME)

固相微萃取技术的萃取效率及应用范围主要取决于其涂层的选择。传统的固相微萃取涂层热稳定性、使用寿命都不理想,溶胶凝胶技术的引入不但增加了涂层的种类,而且增加了使用寿命,提高了其使用温度及抗溶剂冲洗能力,大大拓宽了固相微萃取技术的应用范围。Stationary phase is the key to determine the extraction efficiency and the range of application of SPME. The traditional coatings of SPME are unstable at high temperature. The sol-gel technology can overcome the typical drawbacks of SPME coating, increase its anti-solution ability and thermal stability and broaden its application scope.国家"863"资助项目(编号:2002AA639390

An Orthogonal Expansion Algorithm of Principal Component Suitable to Deal with the Fingerprinting Data of Chinese Medicine

中药指纹图谱数据具有变量数很大而样本数较小的特点,本文中采用拉格朗日求极值的方法得到一种新的适合用于处理这类数据的主成分正交分解算法.结果表明:所得到新的算法,在处理中药指纹图谱数据时,与传统的主成分分析算法比较,节省存储单元,计算量小,计算速度快,因而计算效率高.The fingerprinting data sets of Chinese medicine are the data sets with large number of variables and few objects.A new kind of orthogonal expansion algorithm of Principal Component that is suitable to deal with this kind of data sets has been obtained by use of the Lagrange method of solving extremum problem in this paper.The results indicate that by comparing with the traditional Principal Component Analysis algorithm the new presented algorithm is memory-saving,with small amount of calculation,fast and effective when dealing with the fingerprinting data of Chinese medicine or the data with large number of variables and few objects.福建省自然科学基金(C0210006);; 福建中药GAP关键技术研究基金(2002Y024)资

Rapid Quality Control of Licorice in Its GAP Research

目的　建立甘草 GAP过程中的快速质量检验方法 ,为甘草药材的快速质量检测提供方法依据。方法　提出甘草中水溶性有效物质群的概念并建立其含量的比色测定方法。以甘草酸作为定量的标准物质 ,采用香草醛 -浓硫酸试剂作显色剂 ,用便携式小型光谱仪于 5 6 0 nm处检测。结果　回归方程为 Y=1.174 7C+0 .0 873,相关系数 r=0 .970 5 (n=3) ,回收率为 92 %～ 99% ,在 0 .0～ 0 .96 mg/m L 范围内仪器读数与甘草酸浓度呈线性关系。结论　该方法简单、快速、廉价 ,能够准确地反映甘草质量的优劣 ,适合在准确度要求相对较低的甘草生产基地推广使用Objective To develop a rapid method for the quality control of licorice in its GAP research.Methods Water-soluble triterpenoid saponins were defined as the active fraction in licorice and a colorimetric method using LED-based portable device has been developed for the first time to measure the content of this active fraction. The method was based on the specific color reaction occurring between triterpenoid saponins and vanillin-sulfuric acid reagent. Visible light absorption of 560 nm was chosen as the detection wavelength.Results The operating calibration curve(Y=1.174 7C +0.087 3 mg/mL) was found to be linear at the range of 0.0～0.96 mg/mL glycyrrhizic acid in water (r=0.970 5). The recovery is 92～99%.Conclusion The method is simple, rapid and low-cost and is recommendable to evaluate the quality of Glycyrrhiza uralensis Fisch. in its GAP research.内蒙梁外甘草 GAP研究与开发;; 国家自然科学基金 2 0 0 3重点项目 ( 2 0 2 3 5 0 2 0

The study on determination of trace elements and transference characteristics in the botanic chinese medicinal herb of reducing blood sugar and health food

目的 :对植物性降血糖中药及保健食品中微量元素的含量及溶出特性进行研究 ;方法 :电感耦合等离子体质谱法 (ICP -MS) ;结果 :不同的降血糖中药和保健食品的消解液及冲泡液中锰、铁、锌、钙的含量都很高 ,铜、镍、硒次之 ;其中BCBT茶中镍的溶出率最高达 6 0 2 % ,铜、锌次之 ,分别为 38 7%、35 1%。objective: studying the determination of trace elements and transference characteristics in the botanic chinese medicinal herb of reducing blood sugar and health food; methods: Inductively Coupled Plasma Mass Spectrometry(ICP-MS); results: in different chinese medicinal herbs of reducing blood sugar and health food ,the contents of Mn?Fe?Zn?Ca are very high, followed by Cu?Ni?Se and the extractive content of Ni in BCBT tea is the highest :60 2% ,Cu Zn is second: 38 7%?35 1%.福建省青年科技人才创新项目 ( 2 0 0 1J0 63

Application of pattern recognition technology in classification of Radix et Rhizoma Glycyrrhizae of different sources

目的:建立不同来源甘草药材的模式识别分类方法。方法:通过 HPLC 快速获得19个不同来源甘草药材样品的色谱指纹图谱,色谱条件固定相为 Kromasil KR100-5 C_(18)(150mm×4.6mm),流动相为乙腈-0.05%三氟乙酸溶液,梯度洗脱为乙腈20%(0min)→40%(5min)→50%(10min),流速为0.8mL·min~(-1),检测波长为254nm,从每个色谱指纹罔中提取出325个特征变量,采用聚类分析对甘草药材样品进行相似性评价,并应用 PLS 方法建立起不同植物种、不同种植方式甘草的2个分类回归模型。结果:采用分类模型对不同植物种、不同种植方式甘草进行判别,2个分类回归模型的分类准确率均为100%。结论:此方法可用于不同来源甘草药材的分类研究,本文以 HPLC 指纹图谱结合化学计量学知识,为不同中药样品的质量评价提供了一种分类方法。Objective:To establish a method for pattern recognition classification on Radix et Rhizoma Glycyrrhizae of different sources.Methods:HPLC system was applied to obtain the chromatograms of the 19 Radix et Rhizoma Glycyrrhizae samples.The Kromasil KR100-5 C_(18)(150 mm×4.6 mm)column was used.A mixture of acetonitrile 0.05% trifluoroacetic acid solution was used as the mobile phase with a flow rate of 0.8 mL·min~(-1) and the gradi- ent mode was acetonitrile 20%(0 rain)→40%(5 min)→50%(10 min).The detection wavelength was 254 nm. The 325 characteristic variables were obtained from each chromatogram.The clustering analysis was applied to eval- uate the similarity of the chromatograms.Then partial least-squares regression method was applied to build the pre- diction models of classification which were used to distinguish Radix et Rhizoma Glycyrrhizae of different species and cultivation modes.Results:The classification accuracy of the two prediction models of classification was 100% for Radix et Rhizoma Glycyrrhizae of different sources.Conclusion:This method is practicable in the pattern recog- nition classification on Radix et Rhizoma Glycyrrhizae of different sources.The developed technique could be further applied to the classification of different traditional Chinese medicine(TCM).福建省自然科学基金(C021006);; 福建 GAP 关键技术研究(2002Y024

Determination of trace elements in seawater and application for identification of source of trace metal contaminants

利用电感耦合等离子体质谱(ICP-MS)研究了胶州湾及莱州湾这两个海域中痕量元素污染水平,发展了ICP-MS海水环境中痕量元素的测定方法,同时找出海水环境中具有保守性的数种元素作为污染示踪元素。达到对于海水环境中痕量污染物被动示踪的目的。对18个真实样品进行了识别率试验,识别率可达90%以上,在选取3个海水样品及1个河水样品混合后的模拟分担率实验,也取得了满意的结果,其误差平均值仅有1.17%。Inductively coupled plasma-mass spectrometry(ICP-MS) was developed into an accurate and sensitive technique for the multi-element determinations in a range of sample matrices.The seawater samples in Lai zhou Bay and Jiaozhou Bay as a case was studied.The distribution of trace elements in seawater can be used in the source fingerprints for the identification of seawater samples from different locations.The probability of success for the source identification by the technique is better than 90%.The feasibility of trace metals in seawater as a tracer for the tracking of pollution sources has been evaluated.Combined with the chemo-metric analysis,3 seawater and 1 river samples were mixed,the error is only 1.17%.国家863项目(2005AA635250

Determination of Carthamin in Safflower(Carthamus tinctorius L)by RP-HPLC

经从红花 (CarthamustinctoriusL)中分离纯化、HPLC检测、质谱鉴定得红花红色素纯品 ,并用其作为标准品 ,采用反相高效液相色谱法 ,测定了不同产地红花和商业红花产品中红花红色素的含量。该方法准确性高、重现性好 ,平均回收率为98.1%。The carthamin,extracted from the safflower(Carthamus tinctorius L),was purified and identified byMS.Itwas then used as a standard for the reversed phase high performance liquid chromatographic determiˉnation of carthamin in safflower collected fromdifferentareas and in commercial safflower products.HPLC sepˉaration was carried out on an Alltima C 18 column(5μm,150×4.6mm)with a mixture of acetonitrile,methanol and water(30∶10∶60by volume)at pH=3as mobile phase.The linear range was0.05～0.2g/Lwith a correlation coefficient of0.999.The average recovery and RSD were98.1%and1.9%,respecˉtively