微波超声波联用萃取白藜芦醇及其苷的HPLC测定

建立了花生芽和葡萄籽微波超声波联用提取白黎芦醇及其苷的HPLC测定方法。采用高效液相色谱进行测定,色谱柱为迪马C_(18),流动相为乙腈-水溶液,梯度洗脱,流速1.0 ml/min,柱温为30℃,检测波长为306nm,进样量为20μl。白黎芦醇在0.343～15.15×10~3μg/ml范围内呈良好的线性关系,相关系数R~2=0.9967;白藜芦醇苷在110.712～1774.23×10~3μg/ml范围内线性关系良好,相关系数R~2=0.9993。该方法检测快速、简便、重现性好,适用于花生芽和葡萄籽中白藜芦醇及其苷的定量分析。     

HPLC法测定复方独仲颗粒中芍药苷和绿原酸的含量

建立HPLC法测定复方独仲颗粒中芍药苷和绿原酸的含量。色谱柱为ODS HYPERSIL(250 mm×4.6 mm,5μm);流动相甲醇-0.3%冰乙酸水梯度洗脱,0¹2 min,20∶80,1212 min,20∶80,12²0 min,30∶70;柱温25℃,检测波长绿原酸327 nm,芍药苷230 nm,流速1 m L/min。结果表明,芍药苷和绿原酸在0.031 2520 min,30∶70;柱温25℃,检测波长绿原酸327 nm,芍药苷230 nm,流速1 m L/min。结果表明,芍药苷和绿原酸在0.031 25²μg/m L(r=0.999 7),0.006 252μg/m L(r=0.999 7),0.006 25⁰.4μg/m L(r=0.999 3)浓度范围内呈良好的线性关系。平均回收率分别为98.63%(RSD=0.83%),98.43%(RSD=0.43%)。该方法简便、准确、稳定性好,能有效的控制复方独仲颗粒中芍药苷和绿原酸的含量。     

HPLC-PAD法同时测定维药祖卡木颗粒中甘草苷、柚皮苷、槲皮素和山奈酚的含量

建立采用超声提取、高效液相色谱-二极管阵列检测法测定祖卡木颗粒中甘草苷、柚皮苷、槲皮素和山奈酚含量的方法。色谱柱:安捷伦HC-C18柱(250 mm×4.6 mm,5μm);流动相:乙腈(A)-0.1%磷酸溶液(B),梯度洗脱;检测波长286 nm,365 nm,柱温30℃,流速1.0 m L/min。结果表明,甘草苷、柚皮苷、槲皮素和山奈酚分别在0.2⁴0μg/m L(r=0.999 8)和1.040μg/m L(r=0.999 8)和1.0⁶0μg/m L(r=0.999 9),0.560μg/m L(r=0.999 9),0.5⁶0μg/m L(r=0.999 9)和0.560μg/m L(r=0.999 9)和0.5⁶0μg/m L(r=0.999 8)浓度范围内呈良好的线性关系,平均回收率分别为102.8%(RSD=1.08%,n=5),97.3%(RSD=0.65%,n=5),103.6%(RSD=1.36%,n=5)和101.4%(RSD=1.63%,n=5)。该方法简便、快速、有效、灵敏、准确、具有良好的重复性和回收率,可作为该药物的定量分析方法。     

HPLC法测定制首乌无糖颗粒中二苯乙烯苷的含量

建立HPLC测定制首乌无糖颗粒中二苯乙烯苷的含量的方法。色谱条件为Agilent 5TC-C18(150 mm×4.6 mm,5μm)色谱柱,乙腈-水(27∶73)为流动相,流速1.0 m L/min,柱温25℃,检测波长320 nm,进样量5μL。结果表明,二苯乙烯苷在0.5⁵μg范围内线性关系良好(r=0.999 6),平均加样回收率为102.22%,RSD=1.08%。该方法简便、可靠,适用于制首乌无糖颗粒的质量控制。     

HPLC法测定妇炎舒胶囊中红景天苷的含量

建立妇炎舒胶囊中红景天苷含量的测定方法。采用Welchrom XDB-C18(4.6 mm×250 mm,5μm)色谱柱,0.1%甲酸水溶液-乙腈(83∶17)为流动相,检测波长为275 nm,流速为1 m L/min,柱温30℃,进样体积10μL。结果表明,红景天苷在9.5¹52.1μg/m L范围内具有良好的线性关系(r=0.999 9),平均回收率为100.66%,RSD=1.84%(n=6)。该法简便易行、结果准确、重复性好,可用于妇炎舒胶囊中红景天苷的含量测定。     

超高效液相色谱-串联质谱法检测运动型沐浴露中的泛酸

建立并优化了一种超高效液相色谱-串联质谱法检测运动型沐浴露中泛酸的方法。样品的前处理选择乙醇作为泛酸成分的提取溶剂,并采用T3色谱柱分离,泛酸组分在2.0²00.0μg/L浓度范围内线性关系良好,相关系数r200.0μg/L浓度范围内线性关系良好,相关系数r²为0.999 9,检出限为0.04 mg/kg,定量限范围为0.12 mg/kg,加标回收率为90.7%2为0.999 9,检出限为0.04 mg/kg,定量限范围为0.12 mg/kg,加标回收率为90.7%⁹5.1%。     

HPLC法测定肺胀颗粒中橙皮苷和甘草苷的含量

建立同时测定肺胀颗粒中橙皮苷和甘草苷含量的方法。采用HPLC-UV法,Diamonsil C_(18)柱(4.6 mm×150 mm,5μm),流动相为0.2%磷酸水溶液-乙腈,梯度洗脱,检测波长为283 nm,柱温为30℃,流速为1 mL/min。橙皮苷和甘草苷分别在3.812¹14.36μg/mL和1.874114.36μg/mL和1.874⁵6.22μg/mL范围内线性关系良好,平均回收率分别为100.2%,98.87%,RSD分别为1.45%,1.15%。该法简便、准确、灵敏、重现性好,可用于肺胀颗粒中橙皮苷和甘草苷含量的同时测定。     

采用HPLC法测定温敏水凝胶中白藜芦醇的含量

为建立白藜芦醇温敏凝胶的检测分析方法，采用高效液相法测定温敏凝胶剂型中白藜芦醇的药物质量浓度，选用色谱柱为Waters Symmetry C18(4.6 mm×150 mm,5.0μm)，柱温30℃，流动相为甲醇、水(体积比58∶42)，流速为0.8 mL·min^-1，检测波长为306 nm，进样量为10μL，以保留时间定性、峰面积定量检测白藜芦醇质量浓度。结果表明：白藜芦醇在25～500μg·mL^-1范围内线性程度良好(R²=0.999 4)，稳定性相对标准偏差(RSD)值为1.08%，重复性精密性RSD为1.81%，精密度考察RSD值为1.17%，加样回收率为100.43%(RSD为2.41%,n=9)。该方法具有简便、特异性强、稳定性好、重现度高等优点，可为白藜芦醇温敏凝胶的检测提供依据。     

万源粗榧中高三尖杉酯碱的含量测定

建立了高效液相色谱法测定高三尖杉酯碱含量的方法。采用超声波辅助提取高三尖杉酯碱,利用C18色谱柱,以甲醇∶醋酸铵(53∶47,V/V)为流动相,用二极管阵列检测器(检测波长290 nm)对高三尖杉酯碱进行测定,流速1.0 m L/min,柱温25℃。结果表明,在0.12¹.2 mg/m L的范围内呈良好的线性关系,相关系数R=0.999 94,回收率为97.02%1.2 mg/m L的范围内呈良好的线性关系,相关系数R=0.999 94,回收率为97.02%⁹9.74%。方法操作简便、快速、灵敏度较高,适用于高三尖杉酯碱的测定。     

超高效液相色谱法分离测定环境空气中酚类化合物

建立了分离检测环境空气中酚类化合物的超高效液相色谱法。采用ACQUITY UPLCHSS T3色谱柱进行分离,柱温30℃,以超纯水(含0.5%乙酸)和乙腈(含0.5%乙酸)作为流动相进行梯度洗脱,流速0.2 m L/min,进样量5.0μL,280 nm波长条件下紫外检测;可以实现环境空气中11种酚类化合物的分离测定。结果表明,酚类含量在0.5⁴0μg/m L范围内线性关系良好,相关系数均大于0.999;在采样体积为25 L时,方法检出限范围为440μg/m L范围内线性关系良好,相关系数均大于0.999;在采样体积为25 L时,方法检出限范围为4³9μg/m39μg/m³,相对标准偏差0.39%3,相对标准偏差0.39%⁵.0%,质控样测定相对误差在1.5%5.0%,质控样测定相对误差在1.5%³.8%之间。本方法分离测定环境大气中酚类时准确性好、灵敏度高、操作简便。     

水热法制备石墨烯及对抗坏血酸电催化性能的研究

以氧化石墨烯为前驱液,采用水热技术在碱性环境下合成出水溶性较好的石墨烯。采用扫描电子显微镜技术（SEM）和X射线粉末衍射（XRD）对石墨烯的结构形貌做了表征。采用循环伏安法等电化学测试技术考察了石墨烯电极对抗坏血酸的电催化性能。实验结果表明,抗坏血酸在该石墨烯电极上的电化学活性显著提高。在pH=6.99条件下,峰电流响应最大。在优化条件下,抗坏血酸的响应电流和其响应浓度（1×10^-4~1×10^-3 mol/L）呈较好的线性关系,线性回归方程为I（A）=14 927.87c（mmol/L）+41.19,线性相关系数R²=0.998 9。该检测方法用于维生素C药片的实际测定,与标准测定方法相比,具有较高的准确度。     

Conformation of isotactic polystyrene (IPS) in the bulk crystallized state as revealed by small-angle neutron scattering

Neutron scattering experiments have been performed on isotactic polystyrene (IPS) samples in the bulk crystallized state (T_{crystallization} = 185°C). The determination of the conformation of tagged chains ranging from 2.5 × 10⁵ to 7 × 10⁵ has been undertaken on two different hydrogenated IPS matrices. A matrix of usual molecular weight (M_w = 4 × 10⁵) leads to results which do not agree with Flory's model. In this case, measurements on radius of gyration R_g show on the one hand an important increase of this parameter (40%) with increasing crystallinity for the highest molecular weight tagged chains and on the other hand a variation with molecular weight like M^0.78. These results are interpreted with a schematic model involving a long crystalline sequence incorporated in the monocrystal along the 110 plane and two amorphous wings. Such an assumption is confirmed by the scattering behaviours in the intermediate range. On the other hand, by using an IPSH matrix of very high molecular weight (M_w = 1.75 × 10⁶), and the same tagged chains previously considered, a very weak variation of R_g with increasing crystallinity is observed. This leads to consider in this case Flory's conformation which is corroborated by data obtained in the intermediate range.     

离子色谱法测毛竹竹叶单糖和糖醛酸组成

以离子色谱建立了一种简便、快速、准确测定木质纤维基单糖组成的方法。采用Dionex ICS-5000⁺离子色谱仪，以CarboPAC^TM PA10 (4 mm×250 mm)阴离子交换柱为分离柱，脉冲安培检测器进行检测，氢氧化钠-乙酸钠进行梯度洗脱，同时检测7种常见单糖和2种糖醛酸，结果表明：在各自线性范围内线性关系良好(R²≥0.999 0)，精密度相对标准偏差(RSD)均小于3%，加标回收率98.53%~118.63%，重复性RSD均小于1.16%，检测限为0.01~ 1 mg/L，定量限为0.05~3 mg/L。对竹叶水解液的单糖组成进行了测定，结果表明：竹叶水解液是由阿拉伯糖、半乳糖、葡萄糖和木糖组成，相应单糖的物质的量比为n(阿拉伯糖) : n(半乳糖) : n(葡萄糖) : n(木糖)=2.9 : 0.7 : 8.2 : 9.7。说明该方法可用于木质纤维基单糖的检测。     

木薯淀粉磁性微球的结构表征及其对溶菌酶的吸附性能

磁性微球是高分子材料与磁性物质通过一定作用复合而成的一类具有特殊功能的磁性高分子微球。以木薯淀粉为原材料,复合共沉淀法制备的改性磁流体Fe₃O₄,采用两步法(化学交联法)制备木薯淀粉磁性微球。利用傅里叶变换红外光谱仪、X射线衍射仪、同步热分析仪、扫描电镜、激光粒度仪、磁天平等对其性能及结构进行表征并研究其对溶菌酶的吸附行为。通过单因素法考察磁性微球用量、溶液pH值、吸附温度、吸附时间对吸附率的影响,并采用准一级动力学模型和准二级动力学模型研究其吸附动力学。结果表明:制备的木薯淀粉磁性微球Fe₃O₄含量为19.71%,D₅₀(中位径)为15.40μm,磁化率为1.571×10^-3cm³/g,形貌规整;在微球用量为1.25g,溶液pH=10,吸附温度为25℃,吸附时间为80min时,微球对溶菌酶的吸附率最高,达到84.67%。以相关系数R²为参考,准二级动力学模型(R²=0.99993)较准一级动力学模型(R²=0.99174)、颗粒内扩散模型(R²=0.69996)能更好描述木薯淀粉磁性微球对溶菌酶的吸附行为。     

A comparison of the attachment of the decay products of radon-220 and radon-222 to monodispersed aerosols

The adsorption of radioactive aerosols is of prime importance when assessing the hazard of inhalation of radioactive materials, especially in the uranium mining industry. In previous studies of the attachment rate, contradicting results on the dependence on particle size have been found. The attachment rate for the attachment of the decay products of Rn-222 to monodispersed polystyrene aerosols (of a diameter from 1.2 to 5.3 μm) in the concentration range 1–67 particles cm⁻³ was measured directly. This is compared with the attachment rate of radon-220 decay products which was measured in a previous experiment. As before, the attachment between the radioactive atoms and the aerosols was found to be directly proportional to the particle concentration N, as well as to the square of the particle radius R.

The attachment coefficient of 4.1 × 10⁵ R² cm³ min⁻¹ and the sticking probability of 0.13 for Rn-222 decay products were found to be larger than that for the decay products of Rn-220 (2.4 × 10⁵ R² cm³ min⁻¹ and 0.08, respectively). The mechanism for the attachment, however, is the same.     

The ratio of the extinction coefficient to the mass of atmospheric aerosol particles as a function of the relative humidity

The ratio R_K of the extinction coefficient of aerosol particles in cm ¹, at the wavelength of light λ = 0·55 μm, and the mass of atmospheric aerosol particles in gem³ has been computed as function of the relative humidity for six types of continental and maritime aerosols. With the mean value R_K = 10⁴ cm²/g for all aerosol types being assumed to be independent of relative humidity, only the order of magnitude of the aerosol mass can be determined from visibility observation or measurement of the extinction coefficient of the aerosol particles.     

马来酸噻吗洛尔眼用凝胶的含量测定

建立一种马来酸噻吗洛尔眼用凝胶中噻吗洛尔的含量测定方法。以C18柱为分析柱,以水（1‰三乙胺,用磷酸调节pH值至5．0）-甲醇（60：40）溶液为流动相,检测波长为295nm,柱温为室温,外标法测定,线性范围为0．05--2．0mg·mL^-1,线性方程为A=1．442×10^7c＋1．809×10^4,r=1．000,回收率为99．74％,RSD为0．44％。本法简单、快速、准确,可用于马来酸噻吗洛尔眼用凝胶的含量测定。     

藻渣热解特性及动力学分析

通过热重实验研究N₂气氛下升温速率对索氏提脂后的小球藻热解特性的影响,利用管式炉在N₂气氛下快速热解实验得出：在400℃时,小球藻热解转化率最高,生物油产率达57.6%,热解气为10%。采用等转化率方法FWO和KAS法对藻渣热解动力学进行分析和比较,结果表明：藻渣热解的主要热解阶段为25~800℃,可分为3个阶段,藻渣的DTG曲线存在两个失重峰,且随着升温速率提高,TG和DTG曲线都向高温区偏移,最大失重速率和残余固体质量都增加。N₂气氛条件下藻渣的主要热解阶段表观活化能和指前因子分别为228.46 kJ/mol和2.49×10²¹ min^-1,此阶段下FWO法和KAS法均能很好模拟藻渣热解数据,线性拟合相关系数（R²）均在0.96以上,最佳热解函数为dα/dT=2.49×10²¹/β exp（-228.46/（RT））（1-α）⁸。     

基于邻二氮菲-Fe2+的间接显色光度法检测片剂中的卡托普利

卡托普利还原Fe³⁺,Fe²⁺与邻二氮杂菲显色物在510 nm处有最大吸收,吸光度(A)与卡托普利浓度有相关性。结果表明,卡托普利浓度(c)在1×10^-6~1×10^-4 mol/L范围内与A呈良好的线性关系:y=0.006 4c+0.005 5,相关系数(r)=0.997 6,检测限为9.37×10^-7 mol/L。该方法用于片剂卡托普利测定,结果满意。     

Estimation of the contribution of tube renewal in the terminal relaxation of linear polybutadiene

A set of low-molecular-weight (low-MW) entangled linear polybutadienes with molecular weights between 1.1 × 10⁴ and 2.5 × 10⁵ have been dilutedly embedded in a high-molecular-weight linear polybutadiene (M_w = 7.6 · 10⁵) matrix. The viscoelastic properties of these blends with 9.1% low-MW polymer have been measured. The loss moduli-frequency master curves, G^″ (Щ), contain contributions from both polymers. The contribution of the low-MW polymer is obtained by subtracting the contribution of the matrix. The maximum in G^″, G^″_m, due to the low-MW polymer occurs at a lower frequency (0.3 to 0.5 log units) than in the homopolymer. This result indicates that the longest relaxation time of the entangled linear polymer embedded in a high-molecular-weight matrix is increased by a factor of 2.0 to 3.0 because tube renewal normally operating in the homopolymer is almost completely absent in the matrix. The longest relaxation time of the polymers in the matrix depends on M^3.3₀. This is only slightly less than the dependence found in linear polymer melts (M^3.3₇). This indicates that reptation and chain-end fluctuation together contribute to the relaxation of linear polymers in permanent networks.