高压消解-火焰原子吸收光谱法测定大米中痕量铅铬镉镍和钴

采用高压溶样弹，将样品用硝酸－过氧化氢溶解后，用FAAS法对大米中铅、铬、镉、镍和钴测定，回收率为96％－103％，RSD分别为2.7%、3.1%、4.3%、3.9%和1.8%。应用于出口大米检测，取得满意的结果。     

气相色谱法测定大隆毒饵中的甘氟和氟乙酰胺

用气相色谱法对大隆毒铒中的甘氟和氟乙酰胺进行了联合分析。毒铒用索氏提取器提取，以异丙醇为内标，在GDX-102色谱柱上进行分离，氢焰离子检测器。方法的平均回收率分别为：甘氟Ⅰ：98.3%,甘氟Ⅱ：97.7%，氟乙酰胺：98.2%，相对标准偏差分别为1.0%，1.5%，1.0%（n=10)。     

门源茶Biao果实中脂肪酸分析

用超临界萃取技术对青藏高原藏药特有植物门源茶Biao果实中脂肪酸进行萃取，用毛细管气相色谱进行分离和分析，结果表明不饱和脂肪酸在90％以上，其中亚油酸为36.48%，r-亚麻酸为4.5%,α－亚麻酸为29.26%。     

F-T柴油在直喷式柴油机中燃烧与排放特性的研究

煤通过Fischer-Tropsch (F-T)合成可得到十六烷值高、硫和芳香烃质量分数极低的F-T柴油。研究分析了未作改动的单缸直喷式柴油机燃用F-T柴油时的燃烧和排放特性。结果表明，与燃用0号柴油相比，燃用F-T柴油时的滞燃期平均缩短18.7%，预混燃烧放热峰值降低26.8%，扩散燃烧放热峰值较高，燃烧持续期相当。燃用F-T柴油时的最高燃烧压力略低，最大压力升高率显著下降，机械损失和燃烧噪音较小，燃油消耗率和热效率都得到显著改善。燃用F-T柴油可同时降低CO、HC、NOx和炭烟排放，其中NOx和炭烟分别平均降低16.7%和40.3%。研究表明，F-T柴油是柴油机良好的清洁代用燃料。     

气相色谱法测定化妆品用原料及润肤油中角鲨烷

建立气相色谱法测定化妆品用原料及润肤油中的角鲨烷含量的方法。将化妆品用角鲨烷原料用正己烷溶解；将0.3 g含角鲨烷的润肤油加入皂化液，于75℃振荡水浴下皂化40 min后用正己烷萃取。设置分流比为10∶1,220℃升温至280℃区间升温速率设为5℃/min，然后用外标法分别对样品中的角鲨烷含量进行分析。角鲨烷质量浓度在10～500μg/mL范围内标准曲线线性方程为y=1.933 1x-3.691 4,r=0.999 9，方法检出限为1.7 mg/kg，定量限为5.1 mg/kg。化妆品用原料和润肤油中角鲨烷的加标回收率分别为96.1%～107.2%、92.2%～96.8%，测定结果的相对标准偏差小于1.5%(n=6)。     

火焰原子吸收光谱法测定钼精矿中铜铅铁钙

试样以盐酸和硝酸分解，残渣经回升并入原溶液，在稀盐酸介质中，用火焰原子吸收光谱法测定铜、铅、铁和钙，回收率在95.0%～105.0%,RSD分别为1.7%,1.9%,1.9%和4.2%。     

离子色谱法分析布洛芬片剂的布洛芬含量

研究离子色谱分析布洛芬片剂中的布洛芬含量的分析方法。用碳酸钠-碳酸氢钠溶液作为淋洗液，并以此淋洗液作为提取液，提取布洛芬片剂中的布洛芬，用紫外检测器在波长215nm下检测。回收率在96%-98%之间，RSD等于0.92%，方法简单快速。     

液相色谱法测定鳗鱼中的孔雀石绿

用高效液相色谱法测定鳗鱼组织中孔雀石绿的残留量。鱼体中残留的孔雀石绿在酸性介质下，经高速均质后，用乙腈均质提取，合并提取液，用二氯甲烷再次萃取，有机相过无水硫酸钠和氧化铝复合小柱后浓缩至干，用盐酸羟胺和流动相定容。以乙酸盐缓冲溶液和乙腈为流动相，在KR60－5氰柱上分离后，用可见光检测器在618nm处测定吸光强度，外标法定量。其检出限为1μg/kg，回收率为93.5%-99.6%，相对标准偏差RSD为6.54%-11.0%。     

微波消化-石墨炉原子吸收法测定食用油脂中的铜

用微波消化技术对各种食用油脂试样进行预处理，针对样品特性，优化较佳的微波消化条件与操作参数，建立了用微波消化－石墨炉原子吸收法测定食用油脂中的铜，减少了样品处理过程中的损失，回收率为92.4%-96.2%；RSD为3.0%-3.6%, 检出限为0.05mg/kg。     

高效液相色谱法测定水产品中的恶喹酸

建立了高效液相色谱法测定水产品中恶喹酸残留量的方法。样品用二氯甲烷提取后，除去溶剂，用稀盐酸和正己烷处理，去除残渣中的脂肪，再用二氯甲烷萃取，浓缩至干后用甲醇定容。以0.002mol/L磷酸溶液－乙腈－四氢呋喃（体积比为65：20：15）为流动相，在ODS反相色谱柱上分离后，用荧光检测器测定，外标法定量。方法的线性范围为5－5000ng/mL，线性回归方程为A＝9.426c-2.123，相关系数r=0.9988，检出限为1μg/kg，回收率为93.0%-96.0%，相对标准偏差为3.7%-6.2%。     

Evaluation of analytical reporting errors generated as described in SW-846 Method 8261A

SW-846 Method 8261A incorporates the vacuum distillation of analytes from samples, and their recoveries are characterized by internal standards. The internal standards measure recoveries with confidence intervals as functions of physical properties. The frequency these confidence intervals include true values was very close to theoretical predictions. The ruggedness of the Method’s generation of confidence intervals was tested by analyzing water samples that were altered using salt, glycerin, oil, and detergent, and by increasing sample volume. Quality-control requirements were established for identifying when results might not be normally distributed. There were 11,260 analyte results, of which 90.8% of the data passed quality controls. Their distribution about true value was near theoretical values (71.3, 95.0, and 99.2% for one, two and three sigma deviations). Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

新型FIA光度法测定铝合金中的铜

研制出了一种新的流动比色装置(FIA),不需要增加任何辅助设备,一次进样同时可连续获得两峰一谷3个吸光度值,均可以用于定量分析.利用吸光度加和技术,使分析装置的灵敏度得到大幅度的提高.对其理论扣实验技术进行了研究和尝试,并用于铝合金中铜的测定,实验结果令人满意.     

Characterization of the raw essential oil eugenol extracted from <Emphasis Type="Italic">Syzygium</Emphasis> <Emphasis Type="Italic">aromaticum</Emphasis> L.

Eugenol is the main volatile compound extracted oil from clove bud, Syzygium aromaticum L., and used in traditional medicine, as a bactericide, fungicide, anesthetic, and others. Its extraction was performed using hydrodistillation which is the most common extraction technique. Its components and thermal behavior were evaluated using gas chromatography (GC) and differential scanning calorimetry (DSC), which provide a better characterization of these natural compounds. This extracted product was compared to the standard eugenol results. The GC results suggested ~90% eugenol was found in the total extracted oil, and some of its boiling characteristics were 270.1 °C for peak temperature and 244.1 J g⁻¹ for the enthalpy variation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

混合稀土储氢合金中氧和氮的测定

研究了混合稀土储氢合金中氧和氮的测定方法。针对稀土金属高温易挥发、分解的特点，选择适宜的加热温度，使用镍浴，选择高温座坩埚进行试验：选择出了合适的助熔剂的预处理方法。方法已用于实际样品。对含氧0．43％、含氮0.018％的试样，分析精密度为氧4．3％，氮5.9％，加标回收率氧为93％～104％，氮为92％～110％。     

Pattern recognition methods as supplementary techniques for identification of salicylamide — cyclodextrins inclusion complexes

The objective of this study was to learn whether or not the pattern recognition methods, such as agglomerative cluster analysis (CA) and principal component analysis (PCA), can be used as supplementary techniques for identification of salicylamide (SAA) inclusion complexes with β-cyclodextrin (β-CD) and 2-hydroxypropyl-β-cyclodextrin (HP-β-CD). To do this, phase-solubility of SAA in the presence of the cyclodextrins was studied by the Higuchi-Connors method, which showed that the cyclodextrins enhanced the solubility of SAA in water as compared to that of the drug. Next, the solid phase complexes of the drug with β-CD and HP-β-CD were prepared by using the coprecipitation, precipitation-evaporation, and kneading methods. Identification of the inclusion complexes was performed by using thermal analysis, infrared spectroscopy, and wide angle X-ray scattering. Two multivariate statistical methods, CA and PCA, were used as the supplementary techniques for identification of the inclusion complexes. The results of the statistical analysis have shown that CA and PCA are helpful for interpretation of the thermoanalytical and spectral data. Moreover, these methods enabled proper classification of the products in all doubtful cases. They can be used as supplementary techniques to verify the conclusions of the above-mentioned standard methods.      

灭多威和马拉硫磷复配制剂的气相色谱分析方法

采用气相色谱法 ,在 5 %SE 3 0ChromosorbWAW DMCS (60～ 80目 )色谱柱上 ,测定灭·马乳油中灭多威和马拉硫磷的含量。其相对标准偏差分别为 0 .1 4% ,0 .2 8% ;回收率分别为99.7% ,97.0 %。方法用于产品质量检测 ,结果满意     

Effect of Supplementary UVB Radiation on Chlorophyll Synthesis and Accumulation of Photosystems during Chloroplast Development in Spirodela oligorrhiza

Abstract— Although the effects of ultraviolet B (UVB, 290–320 nm) radiation have been studied in plants extensively, little is known about the potential impacts on maturation of chloroplasts. To address this problem, the effects of supplementary UVB on chloroplast development were examined in the aquatic higher plant Spirodela oligorrhiza. Dark-grown Spirodela-containing proplastids were exposed to photosynthetically active radiation (PAR) and ultraviolet A (UVA, 320–400 nm), plus supplementary UVB equivalent to 1% of PAR on a photon basis. The biosynthesis and assembly of chlorophyll (Chi) into reaction centers was followed for 4 days in situ by low temperature (77 K) Chi fluorescence. Impacts on chloroplast development were detected after only 1 h incubation in light with supplementary UVB. Fluorescence emission signals from Chi associated with the photosystem (PS) II antenna, PSII reaction centers and PSI reaction centers were detected at the same time with or without UVB, but the magnitude of PS fluorescence was diminished up to 60% in plants incubated in UVB. The Chi content was also lower in UVB-treated plants, but to a lesser degree than anticipated by low temperature fluorescence, suggesting lack of organization and/or association of Chi with PS. Electron transport, measured with room temperature fluorescence induction, was not consistently different in plants exposed to UVB. These results suggest that with UVB, fewer and/or smaller PS form during chloroplast development, but there is not a large inhibition of Chi synthesis or PSII activity.     

PLS紫外分光光度法同时测定复方阿斯匹林三组分含量的研究

复方阿司匹林(APC)是常用的解热镇痛药物,片剂中乙酰水杨酸,咖啡因,非拉西丁的同时测定方法有线性最小二乘法[1],系数倍率法[2]等,由于APC三组分中咖啡因的含量相对较少往往使测定值有较大偏差。本文利用乙酰水杨酸易水解的性质,加入NaOH溶液使之完全水解为水杨酸钠间接求得乙酰水杨酸含量,同时在浓度校正及样品测定时适当增加咖啡因浓度而使各组分浓度差别减小,利用PLS法测定三组分含量。1　PLS法分析原理偏最小二乘法(PartialLeastSquares简称PLS)是一种多组分同时测定的新计算方法。与双波长分光光度法[3],线性规划法[4]比较,它…     

Fourier transform infrared spectroscopy supported by multivariate statistics in compatibility study of atenolol with excipients

The objective of this study was to use Fourier transform infrared spectroscopy (FTIR) and multivariate statistics to investigate compatibility/incompatibility of atenolol as a representative of active pharmaceutical ingredients and excipients, such as β-cyclodextrin, methylcellulose, starch and chitosan, when used in solid dosage formulations. Two-component physical mixtures consisting of atenolol and selected excipients were studied by FTIR spectroscopy and two methods of multivariate statistical analysis – principal component analysis (PCA) and cluster analysis (CA), which were used as a supplementary tool for interpretation of the FTIR spectra. Taking into account variability explained by the first two principal components, the results of PCA were visualized in the form of a bi-dimensional scatterplot. A lack of interaction was confirmed by two distinct clusters created by both atenolol and a particular excipient with their mixtures. In the case of CA, lack of interaction between both ingredients was also indicated by two large clusters at a level of 33 or 66% of the maximum distance. The results of the investigations show that with the exception of β-cyclodextrin, the remaining excipients are compatible with atenolol. These findings were confirmed by complementary methods, such as differential scanning calorimetry, thermogravimetry and X-ray powder diffraction.     

FTIR漫反射光谱法定量分析胶囊中头孢氨苄的含量

采用漫反射红外定量分析技术测定胶囊中的头孢氨苄，可排除辅料的影响，且吸光度与头孢氨苄的质量分数成良好的线性关系，平均回收率为98．9％，RSD为1．6％。