牛血清白蛋白共振瑞利散射和共振非线性散射法测定硫酸软骨素

在pH=2.8～4.0的BR缓冲溶液中,硫酸软骨素(CS)由于磺酸基离解而成为带多个负电荷的大阴离子,而低于其等电点(pI=4.7)的牛血清白蛋白(BSA)则以带正电荷的大阳离子存在,两者之间可结合形成复合物.此时将引起共振瑞利散射(RRS)显著增强,并产生新的RRS光谱,其最大散射波长位于304 nm处.与此同时,它的二级散射(SOS)和倍频散射(FDS)也明显增强,且最大SOS和FDS分别位于471 nm和292 nm.散射增强的强度(△I_(RRS)、△I_(SOS)和△I_(FDS)与CS浓度在一定范围内成正比,可用于CS的定量测定.对于CS的检出限(3σ)分别为2.0 ng/mL(RRS),2.9 ng/mL(SOS)和13.2 ng/mL(FDS).研究了适宜的反应条件,考察了共存物质的影响,表明方法有较好的选择性,可用于市售滴眼液中硫酸软骨素含量的测定.

Abstract：

In a Britton-Robinson (BR) buffer solution of pH 2.8--4.0, chondroitin sulfate (CS), which carries negative charge by the ionization of sulfonie group, reacted with bovine serum albumin, which car-ries positive charge through electrostatic force and hydrophobic interaction, to form a complex, resulting in a significant enhancement of resonance Rayleigh scattering (RRS) and the appearance of a new RRS spectrum with the maximum wavelength at 304 nm.At the same time, the second-order scattering (SOS) and frequency-doubling scattering (FDS) were enhanced obviously with a peak at 471 nm and 392 nm, re-spectively.The intensity of scattering (△I_(RRS), △I_(SOS) and △I_(FDS)) was directly proportional to the concentra-tion of CS in a certain range.When used in CS determination, this method exhibited high sensitivity, with a detection limit of 2.0(RRS), 2.9(SOS) and 13.2(FDS) ng/mL.The optimum conditions for the reac-tion and the influencing factors were investigated.The interference of foreign substances was examined and this method showed a good selectivity.The method can be applied satisfactorily to the determination of CS in eye drops.     

硫化镉量子点-硫酸依替米星体系的共振瑞利散射和共振非线性散射光谱研究及其分析应用

在弱酸介质中,硫化镉量子点(CdS-QDs)与硫酸依替米星(ETM)在静电引力和疏水作用力下,形成粒径更大的聚集体,导致共振瑞利散射(RRS)、二级散射(SOS)和倍频散射(FDS)显著增强,其最大散射峰分别位于310 nm(RRS),568 nm(SOS),320 nm(FDS).在一定范围内ETM浓度与三种散射增强程度(△I)成正比,可用于ETM的测定,其中RRS的灵敏度最高,其检出限(3σ)为1.6 ng/mL.考察了共存离子的影响,表明方法有良好的选择性.据此发展了以CdS-QDs作探针,高灵敏、简便测定ETM的共振瑞利散射新方法,用于人血清和尿样中ETM的测定,平均回收率在94.5%～113.7%之间.

Abstract：

In a medium of pH = 5.6, CdS quantum dots could react with etimicin sulfate to form larger aggregates by virtue of electrostatic attraction and the hydrophobic force, which resulted in a great enhancement in resonance Rayleigh scattering (RRS) and resonance non-linear scattering such as second-order scattering (SOS) and frequency doubling scattering (FDS). The maximum scattering peaks were located at 310 nm for RRS, 568 nm for SOS and 320 nm for FDS. The enhancements of scattering intensity (△I) were directly proportional to the concentration of etimicin sulfate (ETM) within a certain range. Of the three methods, RRS had the highest sensitivity, its detection limit (3σ) being 1.6 ng/mL. An examination of the effects of coexisting substances showed that the method had good selectivity. Based on these results, a new method, highly sensitive and simple, was developed, which can be used to determinate ETM by CdS-QDs as a probe. The recovery for the determination of ETM in human serum and uric samples was in the range of 94. 5%-113.7%.     

高锰酸钾共振瑞利散射法测定磺胺二甲嘧啶

在0.2 mol/L H_2SO_4介质中,磺胺二甲嘧啶(SM_2)和KMnO_4在加热条件下发生氧化还原反应生成MnO_2微粒,导致共振瑞利散射(RRS)增强,并产生新的散射峰.其最大散射波长位于595 nm附近,散射强度在一定范围内与SM_2的浓度成正比,据此建立了测定SM_2的共振瑞利散射(RRS)新方法.本方法具有较高的灵敏度,检出限为8.6 ng/mL.实验优化了测定条件.考察了共存物质的影响,表明方法具有良好的选择性,用于片剂中SM_2的测定,结果满意.

Abstract：

In 0.20 mol/L H_2SO_4 medium, a redox reaction took place between sulfadimidine (SM_2) and po-tassium permanganate to form MnO_2 particles by heating.As a result, new spectra of resonance rayleigh scattering appeared and their intensities were enhanced greatly.The maximum peak of RRS was located at approximately 595 nm, and the scattering intensities were proportional to the concentration of SM_2.Based on these results, a new method for the determination of SM_2 was established.The detection limit (3σ) was 8.6 ng/mL.The effects of coexistent substances were tested, and the results demonstrated that this meth-od had good selectivity.It has been applied to the determination of SM_2 in tablets with satisfactory results.     

CdTe量子点作探针共振瑞利散射法测定肝素钠

在水相中低温条件下制备了巯基乙胺稳定的CdTe量子点(CdTe QDs).基于肝素钠(Heparin)对巯基乙胺稳定的CdTe QDs共振瑞利散射(RRS)的增强作用,同时二级散射(SOS)和倍频散射(FDS)也相应增强,建立了一种快速、简便、定量测定肝素的新方法,同时讨论了最佳反应条件和影响因素,以RRS为例,在311 nm处,RRS的光谱强度与肝素钠的质量浓度c/(I-I_0)有良好的线性关系(r=0.999 1),线性范围13.5～1000 ng/mL,检出限(3σ)为4.04 ng/mL.可用于血样中肝素钠的测定.

Abstract：

Aqueous cysteamine-capped CdTe quantum dots(QDs) were prepared under low temperature.A simple and rapid quantitative method for heparin determination was proposed, based on the fact that hepa-tin can enhance CdTe QDs resonance Rayleigh scattering (RRS) and the intensities of second-order scatter-ing (SOS) and frequency-doubling scattering (FDS).Factors affecting RRS for detecting heparin with cys-teamine-capped CdTe QDs were studied.At 311 nm, the RRS calibration plot of C/(I-I_0) with concen-tration of heparin was linear in the range of 13.5-1 000 ng/mL with a correlation coefficient of 0.999.The limit of detection (30) was 4.04 ng/mL.     

微量穴醚(2.2.2)测定方法初探

用紫外分光光度法研究微量穴醚(2.2.2)的检测方法,并将该方法用于氟[18F]脱氧葡萄糖中微量穴醚(2.2.2)测定.将适量苯甲醛加入硝酸铅缓冲溶液中配制储备液,使溶液在250 nm检测波长处的吸收曲线为一平台,用储备液和微量穴醚(2.2.2)配制供试液,用紫外分光光度法检测.穴醚(2.2.2)的线性范围为1.0～10.0 μg/mL,相关系数0.999 5,平均回收率为100.5%(n=5),相对标准偏差为2.24%,方法检出限(3d)为0.15μg/mL.该方法用于氟[18F]脱氧葡萄糖中微量穴醚(2.2.2)测定,结果良好.该方法精密度高,准确性好,可用于微量穴醚(2.2.2)测定.

Abstract：

A method for the determination of trace cryptand 222 by ultraviolet spectrometry was researched. As benzaldehyde and complex of lead cryptand 222 possess the same ultralviolet absorbance peak and their maximum absorbance wavelength are both 250 nm, proper amount of benzaldehyde and lead nitrate was added to the citric acid buffer solution (pH=6.4) for preparing storage solution, and the ultralviolet absorbance curve of the storage solution was made a platform about 250 nm detection wavelength.Trace cryptand 222 was added to the storage solution, and trace complex of lead cryptand 222 was detected by ultraviolet spectrometry for quantitative determination of trace cryptand 222. This method kept in good linearity from 1.0 to 10.0 μg/mL of cryptand 222 concentration with a correlation coefficient of 0. 999 5, a recovery of 100.5% (n=5), a relative standard deviation of 2.24% and a limit of quantification of 0.15 μg/mL. This method has been successfully applied in determination of trace cryptand 222 of [18F]-fluorodeoxyglucose with satisfactory results. This method is simple, accurate and suitable for determination of trace cryptand 222.     

钯(Ⅱ)-盐酸吗啉胍螯合物与卤代荧光素染料相互作用的超瑞利散射光谱及其分析应用研究

在pH=4.4～5.0的HAc-NaAc介质中,钯(Ⅱ)与盐酸吗啉胍(Abob)反应形成螯合阳离子,它能进一步与二溴荧光素(DBF)、曙红Y(EY),赤藓红(Ery)阴离子反应形成离子缔合物,引起超瑞利散射(HRS)显著增强.3个三元体系具有相似的光谱特征,最大HRS波长位于390 nm附近.在一定条件下超瑞利散射增强(△IHRS)与Abob的浓度成正比,其线性范围是0.029～3.0μg/mL(DBF),0.14～3.5μg/mL(EY)和0.23～1.9μg/mL(Ery),检出限分别为0.008 6μg/mL(DBF),0.043 μg/mL(EY)和0.069μg/mL(Ery).研究了HRS法的适宜反应条件和共存物质的影响,发展了高灵敏、简便快速测定Abob的新方法,可用于尿样中Abob的测定.

Abstract：

In an acidic medium with pH = 4.4-5.0, palladium (Ⅱ) chelated with moroxydine hydrochloride to form the cation [ Pd (Abob)]2+ , which reacted further with dibromofluorescein (DBF), eosin Y (EY)and erythrosin(Ery) to form ion-association complexes, respectively. As a result, the hyper Rayleigh scattering(HRS) intensities were enhanced greatly. The maximum HRS peak of the three systems was all located at approximately 390 nm. HRS intensity was proportional to the concentration of moroxydine hydrochloride (Abob) in the range of 0. 029-3.0 μg/mL for DBF, 0. 14-3.5 μg/mL for EY and 0.23-1.9 μg/mL for Ery, and their detection limit (3σ) was 0. 008 6, 0. 043 and 0. 069μg/mL, respectively. The optimum conditions of the reaction and the properties of analytical chemistry were investigated. Therefore, a new method for the determination of moroxydine hydrochloride(Abob) by HRS was developed. The method has high sensitivity and good selectivity and has been applied to the determination of Abob in uric samples with satisfactory results.     

Study on HPLC method to determine contents of Schisandrin A and Schisandrin B in Schisandra chinensis extraction

The determination method of Schisandrin A and Schisandrin B in Schisandra chinensis was improved with the high performance liquid chromagraphy(HPLC).The sample was extracted exceedingly in the critical limit of CO 2 .The retention time of Schisandrin A and Schisandrin B was reduced,with methano/water(75:25)as mobile phase.The wavelength for detection was 254 nm. The R2 of standard curve was 0.9998 and the relative standard deviation was 2.31%and 3.17%with the recovery of 96.45%and 97.37%,respectively.The result shows that the rate of veracity of this method is higher and it proves that the determination method of Schisandrin A and Schisandrin B in Schisandra chinensis is a feasible method.     

The Determination of Canthaxanthin in Feed Ingredients by High Performance Liquid Chromatography

A series of studies were conducted to establish a methodology for the accurate and efficient determination of canthaxanthin in feed ingredients. Agilent ZORBAX Eclipse DB-C 18 analytical column （4.6×150 mm, 5μm） was used and kept at 25 ℃. The mobile phase was acetonitrile ： methanol （v/v）=95 ： 5, and eluted compounds were detected by DAD absorbance （470 nm）. The flow rate was maintained at 1.0 mL·min^-1. The response of the method was linear over the range 1.0-20.0 μg·mL^-1 canthaxanthin assay solution （R^2=0.9998）. Recovery assays done with standard canthaxanthin to feed ingredient resulted in an average recovery of 103%. Variation coefficient was less than 3.53%. This method is proved to be simple, precise, sensitive and reproductive.     

Pretreatment of Rice Straw by Hydrogen Peroxide for Enhanced Methane Yield

A pretreatment process for hydrogen peroxide (H2O2) was optimized to enhance the biodegradation performance of rice straw and increase biogas yield. A determination experiment was conducted under predicted optimal conditions. Optimization was implemented using response surface methodology. The effects of biodegradation and the interactive effects of pretreatment time (PT), H2O2 concentration (HC), and substrate to inoculum ratio (S/I) on methane yield were investigated. The lignin, cellulose, and hemicellulose of rice straw were significantly degraded with increasing HC. The optimal conditions for the use of pretreated rice straw in anaerobic digestion were a 6.18-d PT, 2.68% HC (w/w total solid), and 1.08 S/I; these conditions result in a methane yield of 288 mL g-1 volatile solids (VS). A determination coefficient of 95.2% was obtained, indicating that the model used to predict the anabolic digestion process has a favorable fit with the experimental parameters. The determination experiment resulted in a methane yield of 290 mL g-1 VS, 88.0% higher than that of untreated rice straw. Thus, H2O2 pretreatment of rice straw can be used to improve methane yields during biogas production.     

RP-HPLC法测定薏苡中薏苡素的含量

采用HPLC法,以Diamonsil(R)C_(18)为色谱柱,乙睛-水(50∶50)为流动相,流速1 mL/min,柱温25℃,检测波长232 nm,建立了薏苡非种仁部位中薏苡素的高效液相含量测定方法.结果表明:薏苡素在0.096～1.92μg范围内呈良好的线性关系,该方法的平均回收率为99.12%(n=5),相对标准偏差(RSD)为0.89%,用此条件测得成都华西植物园中薏苡全草中薏苡素的含量为8.3078 mg/g.从成分薏苡素和资源综合利用的角度考虑,建议薏苡根、茎和叶可以入药.

Abstract：

To establish an RP-HPLC procedure for determining the content of coixol in the root,stem and leaf of Coixlacryma-jobi L.var.mayuen(Roman.) Stapf. Methods The Diamonsil(R)C_(18) col-umn was used with the mobile phase of acetonitrile-water (50: 50), a flow rate of 1 mL/min, a tempera-ture of 25℃and a wavelength of 232 nm. Results The linear range of coixol was 0.096-1.92μg. The av-erage recovery was 99.12% (n=5, RSD is 0.89 %). Coixol in the herbal of C. Lacryma-jobi L. Var. Mayue in the Botanical Garden of West China was 8.3078 mg/g. Conclusion This method proved to be simple, accurate,well replicable, and suitable for the determination of C.lacryma-jobi L.var.mayuen(Roman.) Stapf.