固相萃取-气相色谱质谱法测定食用油中邻苯二甲酸酯

建立了固相萃取-气相色谱质谱法测定食用油中邻苯二甲酸酯的分析方法。以正己烷为提取剂萃取试样中的邻苯二甲酸酯,样液经中性氧化铝自组装固相萃取柱净化后进行GC/MS测定分析。采用选择离子扫描方式,用外标法进行定量分析。方法的检出限(S/N=3)为1~6μg/kg。在加标水平为50μg/kg时,平均回收率为67.3~107%,相对标准偏差(RSD)为3.6~6.1%;在加标水平为100μg/kg时,平均回收率为67.5~103%,相对标准偏差(RSD)为3.2~6.2%。本方法简便、快速地实现了食用油中邻苯二甲酸酯的检测。     

凝胶色谱净化-气相色谱串联质谱法测定海产品中得克隆残留量

建立了凝胶色谱(GPC)净化、气相色谱-串联质谱(GC-MS/MS)测定海产品中得克隆的方法。得克隆包括syn-DP和anti-DP两种异构体,样品中的得克隆经正己烷/丙酮(1:1,v/v)溶液提取、GPC净化后,GC-MS/MS采用多反应监测模式(MRM)采集数据后进行定性/定量分析。得克隆的加标回收率:syn-DP测定回收率为89.3%~102.5%;anti-DP测定回收率为85.4%~102.1%。syn-DP和anti-DP的检出限分别为0.2μg/kg和0.5μg/kg(S/N=3)。方法的相对标准偏差(RSD)均≤10.0%。采用本方法对采自温州的美国红鱼、中国毛虾,采自台州的鲈鱼,以及采自舟山的大黄鱼进行检测分析,结果上述样品均未检出。     

液相色谱-串联质谱法检测鸡肉中7种糖皮质激素残留量

建立鸡肉中糖皮质激素多残留的液相色谱-串联质谱分析方法。样品经乙酸乙酯提取,正己烷净化,10%乙腈水定容后供高效液相色谱-串联质谱仪(LC-MS/MS)分析,采用C18色谱柱分离,电喷雾离子化负离子方式(ESI-)及多反应监测模式(MRM)进行测定,外标法定量。研究了仪器条件、提取溶剂、净化溶剂等条件对七种目标物分离状况的影响。在优化条件下,该方法在鸡肉样品中泼尼松的的线性范围为0.5~20μg/L,泼尼松龙、甲基泼尼松、地塞米松、氢化可的松、倍氯米松、氢化可的松乙酸盐的浓度范围为0.1~20μg/L,在加标水平1.0~10μg/kg范围内,回收率为83%~104.2%;相对标准偏差为0.92%~4.89%。     

液相色谱-串联质谱法同时测定饲料中矮壮素和缩节胺的残留

本文采用高效液相色谱-串联质谱(HPLC-MS/MS)同时测定饲料中的矮壮素和缩节胺残留。样品先用正己烷脱除油脂,后用缓冲溶液(含0.2%甲酸-0.05mol/L乙酸铵)提取,离心上清液用乙腈沉淀净化后进行测试。结果表明:两种化合物在1.0~50.0μg/L范围内线性关系良好;定量限(S/N=10)矮壮素为0.32μg/L,缩节胺为0.45μg/L;加标回收率为91.7%~94.3%;相对标准偏差3.9%~6.1%;实测有30%的样品中含有矮壮素或缩节胺,含量范围为:矮壮素11.2μg/kg-78.4μg/kg;缩节胺9.7μg/kg-126.6μg/kg。该方法简便、快速、灵敏和准确,适合饲料中这两种农药残留的快速检测和定量分析。     

植物油中苯并(a)芘液相色谱检测方法的研究

本文研究了植物油中苯并(a)芘的高效液相色谱检测法。试样中的苯并(a)芘用丙酮提取,液相色谱-荧光检测器测定,外标峰面积法定量。苯并(a)芘在(0.5~20)ng/m L范围内呈良好的线性关系,3个水平(2.5μg/kg、5.0μg/kg、10.0μg/kg)添加苯并(a)芘的回收率为93.0%~104.4%,相对标准偏差(RSD)为2.9%~3.9%,检出限为1.0μg/kg。此方法简便、快捷,适用于植物油中苯并(a)芘的检测。     

UPLC-MS/MS法测定虾蟹中4-己基间苯二酚的残留量

建立一种超高效液相色谱-串联质谱(UPLC-MS/MS)测定虾蟹中4-己基间苯二酚残留量的检测方法。样品经乙腈超声提取,C18固相萃取柱净化后,UPLC BEH C18色谱柱分离,多反应监测方式测定,外标法定量。结果显示:加标回收率在88.32%~92.08%之间,相对标准偏差RSD≤2.3%;以S/N=3计算,检出限为5.0μg/kg。该法灵敏度好、准确性高、精密度好、检出限低,适用于虾蟹中4-HR微量和痕量残留的测定。     

水产干制品中抗生素残留的液相色谱-串联质谱测定

运用液质联用技术建立了水产干制品中40种抗生素的同时测定方法。含0.1%甲酸乙腈进行提取,考察了不同萃取溶剂及Na2EDTA添加量对目标抗生素回收率影响。目标抗生素在0.1~100μg/kg范围内线性良好;以基底匹配工作曲线进行定量,在高加标浓度下虾仁、鳗鱼干、红娘鱼干的加标回收率和RSD(n=4)分别为40.5%~138.6%和0.4%~19.4%、41.3%~134.5%和1.3%~11.6%、及40.3%~136.7%和0.1%~14.7%,方法检测限在0.1~0.5μg/kg。方法快速、简便,已成功应用于厦门周边常见水产干制品的检测。     

气相色谱法快速测定油脂及加工食品中的BHA、BHT、TBHQ

本文研究了用毛细管气相色谱快速测定油脂及其加工食品中BHA、BHT、TBHQ含量的方法。样品用无水乙醇提取、过滤、浓缩后直接进样测定。结果三种组分加标回收率在94.6%~109.1%之间,相对偏差均小于5.2%,线性范围在10~500μg/ml之间,相关系数均大于0.999,最低检测浓度(以3N计)均小于0.5μg/ml。     

凝胶色谱净化-气相色谱串联质谱法测定猪肉中16种有机氯类农药残留

建立了凝胶色谱(GPC)净化、气相色谱-串联质谱(GC-MS/MS)同时测定猪肉中16种有机氯类农药残留的方法。样品中的待测农药组分经丙酮、正己烷提取、GPC净化去除油脂等杂质,GC-MS/MS采用多反应监测模式(MRM)采集数据后进行定性/定量分析。待测农药的加标回收率在82%～106%之间,方法的相对标准偏差(RSD)≤10.9%,各农药组分的检出限为0.1～0.9μg/kg。     

微波辅助萃取-超高效液相色谱/静电场轨道阱高分辨质谱法快速测定纺织品中有害有机溶剂残留量

建立了1个快速测定纺织品中有害有机溶剂残留量的超高效液相色谱/静电场轨道阱高分辨质谱(UPLC/Orbitrap HRMS)方法,该方法以乙醇为萃取溶剂,100℃下微波萃取纺织品中残留的有害有机溶剂,萃取液直接进行UPLC/Orbitrap HRMS,提取离子色谱峰面积外标法定量。对样品的提取条件、分析条件进行了优化。该方法的定量限为0.5μg/kg~10.0μg/kg。在3个不同加标浓度水平下,方法的平均加标回收率为81.8~94.5%,相对偏差偏差为3.8%~10.5%(n=9)。该方法简便快速,灵敏度高,定量限低,可有效地解决纺织品中残留的有害有机溶剂的快速测定问题。     

Novel terbium-zircon yellow pigment

The incorporation of the terbium oxide into the zircon host lattice in the presence of different types (NaF and LiF) and amounts (2 and 5 wt%) of mineralisers created various shades of yellow at several calcination temperatures with 2 h soaking time. The shade of yellow observed was primarily a lemon yellow, different from existing Pr-Zircon yellow. The pigment powders were characterised using techniques such as XRD, SEM, Particle Size Analysis and Spectrophotometry. From the X-ray diffraction patterns, zircon was found to be the major phase present together with small amounts of un-reacted zirconia. The amount of un-reacted zirconia in each case was calculated using an external standard method. SEM micrographs of the samples indicated growth of the tetrahedral shaped crystals improved on addition of sodium fluoride. The same zircon crystals were observed to form with the use of lithium fluoride as a mineraliser, but the shape of the crystals differed. The average particle size was found to vary between 11–15 m. Stability of these pigment powders was tested in an unleaded commercial transparent glaze. Yellow coloured glazed tiles were produced suggesting that the pigments were stable in the commercial unleaded transparent glaze. Colour measurements were performed on the pigment powder samples and on the coloured glazed tiles.     

The nature of Pr-ZrSiO4 yellow ceramic pigment

Pr-ZrSiO₄ yellow ceramic pigment is believed to be a solid solution of Pr⁴⁺ with the zircon lattice, but studies are poor and scarce. The aim of this paper is the synthesis of Pr-ZrSiO₄ yellow pigment in the presence of NaF by several non-conventional methods and to investigate the nature of the pigment. Results indicate that the formation of Pr-ZrSiO₄ yellow pigment must be explained by two simultaneous mechanisms: formation of a solid solution of Pr in a ZrSiO₄ network and an occlusion mechanism.     

Chemical synthesis of environment-friendly nanosized yellow titanate pigments

As yellow pigments, nanosized rutile structured Ni_0.1W_0.1Ti_0.8O₂ and priderite structured BaNiTi₇O₁₆ have been prepared through pyrolysis of precursor solution containing nickel nitrate, dimethyl tungstate, titanium oxalate, triethanolamine (TEA) for the former composition and barium nitrate, nickel nitrate, titanium oxalate, TEA for the later composition, respectively. In the reaction, TEA acts to minimize the agglomeration in the products through formation of a highly branched polymeric framework, which anchors the metal ions for producing nanocrystalline powders. The rutile and priderite structured titanates obtained on heat-treatment of the precursor powders at 800 °C and 850 °C, respectively, have been characterized by XRD, TGA-DTA, BET surface area measurement, UV-vis spectroscopy, CIE L^*a^*b^* colour parameter measurements, TEM and HRTEM. XRD reveals the purity of the resulting rutile and priderite phases. Their crystallite sizes, average particle sizes and specific surface areas determined from XRD, TEM, and BET surface area measurement are found to be in the range between 25 nm and 30 nm, 25-45 nm and 100-120 m²/g, respectively, for both compositions.     

用磷矿石真空制备黄磷的热力学研究

引入“物质吉布斯自由能函数法”讨论在不同压力下，磷酸钙、二氧化硅与还原剂碳的反应生成黄磷的热力学条件。研究表明在常压下反应在1460K以上发生；真空条件下，压力降到60～6Pa时，反应在1066～984K时就能进行，比常压下降低了446～476K。真空下磷矿石制备黄磷的热力学研究为工艺实验研究提供理论依据。     

Preparation and properties of toughened yellow zirconia ceramics

To obtain the high toughness yellow ceramic, using the Y₂O₃ (5%) stabilized ZrO₂ as main starting material, Al₂O₃ as toughen reagent, NH₄VO₃, V₂O₅ as colorant, and mixed with ball mill, molded with dry press method and two times sintered. By testing the properties and structure of the ceramic, we have optimized the best technical conditions, and the mechanism of toughness and color present has been studied. The result shows that the NH₄VO₃ as colorant is better than V₂O₅, and the color is between X = 0.396–0.412 and Y = 0.402–0.390. The highest bending strength of toughened ZrO₂ ceramics is 1138 MPa, and the fracture toughness is 14.8 MPa m^1/2. The toughen mechanism is that phase transformation of ZrO₂ and the dispersion of toughen reagents, and the color causing is by the colorful ion (V⁴⁺) entered into the zirconia crystals lattice of the ceramic. The text was submitted by the authors in English.     

Identification of yellow dye types in pre-columbian andean textiles

A number of pre-Columbian textiles, most discovered in northern Peru and dating to the Late Intermediate Period (ca. 1050-1200 AD), were analyzed by high-performance liquid chromatography with diode array and mass spectrometric detection (LC-DAD-MS), after extraction of the dyes with formic acid and methanol. The focus of this work was yellow dyes, most of which are present as glycosides of flavonoids and related compounds, with the objective of identifying the plants originally used for dyeing. Two major types of dyes were found in this set of specimens. The first type is characterized by the presence of flavonol 3-O-sulfates (never before reported as being present in dyes) and 3-O-glycosides; this type was probably derived from the plant Flaveria haumanii or a close relative. The second type is characterized by the presence of both chalcone (heretofore not reported in pre-Columbian textiles) and luteolin glycosides, though a specific plant source could not be identified. Two other yellow dye types appeared to be present, but there were not enough examples to allow conclusions to be drawn. Also present in some extracts were various hydroxybenzoic acids, which appear to be oxidation products of the respective unsubstituted flavonol (3-hydroxyflavone) dyes. Most yellow dyes are synthesized in plants as glycosides (or other derivatives), which are incorporated more or less intact into textile fibers during dyeing. Extraction of these derivatives and analysis by LC-DAD-MS yields distinctive profiles that, with appropriate plant reference materials, can aid in the identification of the original plant dyestuffs.     

纳米铁黄的表面改性及表征

研究了纳米铁黄有机表面改性的影响因素，确定了最优改性剂和改性条件。采用红外光谱（IR）、热分析（TG）、透射电镜（TEM）和分散性实验对表面改性前后的纳米铁黄进行了表征。实验结果表明，以硬脂酸为改性剂、用量为5％、pH值为4、改性时间为1．5h时，改性后的纳米铁黄的亲油化度达到92．6％。红外光谱和热分析显示，硬脂酸以化学键合的方式结合在纳米铁黄的表面，其质量分数约为4％。透射电镜（TEM）和分散性实验表明，经硬脂酸有机表面改性的纳米铁黄具有亲油疏水性能，能较好地分散于有机溶剂二甲苯中。     

Controlling the yellow luminescence intensity from n-GaN during cathodoluminescence

GaN grown on sapphire by hydride vapour phase epitaxy is probed by ion channeling, Raman and cathodoluminescence (CL) spectroscopy. Channeling and Raman spectroscopy indicate that the quality of GaN is very good. Spot mode CL measurement signifies intense near band edge emission as compared with yellow luminescence (YL). During scanning over an area, the YL intensity could be controlled by the electron beam dwell time (DT). The YL intensity decreases with the increase of DT and saturates beyond a threshold value due to overexposure of a given pixel leading to non-radiative emission. But for shorter dwell times repeated excitations of a given pixel increase the intensity of YL. These results may be explained invoking the decay time and density of defects responsible for YL. Control over YL intensity will be useful for assessing low defect concentrations, their origin and also to increase spatial resolution of CL measurements on nanostructures.     

高效稳定性有机黄光电致发光器件

主要通过红绿磷光材料R-4B和GIr1掺杂的方法,制备了黄光OLED器件,器件结构为ITO/MoO3(X)/NPB(40nm)/TCTA(10nm)/CBP:GIr1 14%:R-4B2%(30nm)/BCP(10nm)/Alq3(40nm)/LiF(1nm)/Al(100nm),TCTA和BCP分别为电子和空穴阻挡材料,同时结合TCTA和BCP对载流子的高效阻挡作用,研究了MoO3对器件效率和稳定性的影响。发现当增加MoO3的厚度为90nm时,在较大的电压范围内,器件都具有较高的效率和色坐标稳定性。在电流密度为7.13mA/cm2时,器件达到最高电流效率29.2cd/A,亮度为2081cd/m2;电流密度为151.7mA/cm2时,获得最高亮度为24430cd/m2,电流效率为16.0cd/A;器件色坐标稳定性较好,当电压为5、10、15V时,色坐标分别为(0.5020,0.4812)、(0.4862,0.4962)、(0.4786,0.5027)。器件性能的改善主要归因于载流子注入与传输的平衡以及阻挡层对发光区域的有效限定。