大口径毛细管气相色谱法直接测定植物生长激素

采用大口径毛细管气相色谱法对多种植物生长激素进行了测定。萘乙酸（ＮＡＡ）、吲哚－３－乙酸（ＩＡＡ）、吲哚－３－丁酸（ＩＢＡ）、脱落酸（ＡＢＡ）和赤霉素（ＧＡ）５组分,不需衍生化处理,直接进样,获得了良好的分析结果。其ＮＡＡ、ＩＡＡ、ＩＢＡ、ＡＢＡ、和ＧＡ的最低检测限分别为５．２×１０－５、１．２ ×１０－４、１．７ ×１０－４、２．２ × １０－４、８．５ ×１０－４ｇ／Ｌ;其回收率分别为 ９２．４％、９１．８％、９８．２％、８９．７％、９１．４％。方法快速、简便。     

FERROMAGNETIC INTERACTION BETWEEN GADOLINIUM（Ⅲ） AND COPPER （Ⅱ）IONS IN N，N＇－BIS（2－AMINOPROPYL）OXAMIDO COPPER（Ⅱ） BRIDGED BINUCLEAR Gd（Ⅲ）－Cu（Ⅱ） COMPLEX

ＦＥＲＲＯＭＡＧＮＥＴＩＣＩＮＴＥＲＡＣＴＩＯＮＢＥＴＷＥＥＮＧＡＤＯＬＩＮＩＵＭ（Ⅲ）ＡＮＤＣＯＰＰＥＲ（Ⅱ）ＩＯＮＳＩＮＮ，Ｎ＇－ＢＩＳ（２－ＡＭＩＮＯＰＲＯＰＹＬ）ＯＸＡＭＩＤＯＣＯＰＰＥＲ（Ⅱ）ＢＲＩＤＧＥＤＢＩＮＵＣＬＥＡＲＧｄ（Ⅲ）－Ｃｕ...     

CRINISINE，A NEW ALKALOID FROM CRINUM ASIATICUM L．VAR．SINICUM （ROXB．EX HERB）BAKER

ＣＲＩＮＩＳＩＮＥ，ＡＮＥＷＡＬＫＡＬＯＩＤＦＲＯＭＣＲＩＮＵＭＡＳＩＡＴＩＣＵＭＬ．ＶＡＲ．ＳＩＮＩＣＵＭ（ＲＯＸＢ．ＥＸＨＥＲＢ）ＢＡＫＥＲ￥ＲｅｎＪｉｕＴＡＮＧ；ＮｉｎｇｊｉＢＩ（ＧｕａｎｇｘｉＩｎｓｔｉｔｕｔｅｏｆＴｒａｄｉｔｉｏｎａｌＭｅｄ...     

INVESTIGATION ON SIMPLE OSCILLOGRAPHIC VOLTAMMETRY WITH FEEDBACK VOLTAGE

ＩＮＶＥＳＴＩＧＡＴＩＯＮＯＮＳＩＭＰＬＥＯＳＣＩＬＬＯＧＲＡＰＨＩＣＶＯＬＴＡＭＭＥＴＲＹＷＩＴＨＦＥＥＤＢＡＣＫＶＯＬＴＡＧＥ￥ＪｉａｎＢｉｎＺＨＥＮＧ；ＨｏｎｇＧＡＯ（Ｈ．Ｋａｏ）（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，Ｉｎｓｔｉｔｕｔｅ...     

AB INITIO STUDY ON GAS-PHASE FACTION OF Ca WITH HN_3

ＡＢＩＮＩＴＩＯＳＴＵＤＹＯＮＧＡＳ－ＰＨＡＳＥＦＡＣＴＩＯＮＯＦＣａＷＩＴＨ　ＨＮ_３（ＲｏｎｇＳｈｕｎＺＨＵ；ＳｈｕＳｈａｎＤＡＩ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，ＹｕｎｎａｎＵｎｉｖｅｒｓｉｔｙ．Ｋｕｎｍｉｎｇ６５００９１．）ＡＢＩ?..     

THE THERMAL DECOMPOSITION OF BARIUM（Ⅱ） TETRAPHENYLBORATE

ＴＨＥＴＨＥＲＭＡＬＤＥＣＯＭＰＯＳＩＴＩＯＮＯＦＢＡＲＩＵＭ（Ⅱ）ＴＥＴＲＡＰＨＥＮＹＬＢＯＲＡＴＥ￥ＢａｏＸｕｅＺＨＯＵ；ＷｅｉＫｅＺＨＯＮＧ；ＬｉＺｈｕａｎｇＺＯＵ；ＸｉａｏＬｉｎｇＷＡＮＧ（Ｄｅｐｔ．ｏｆＣｈｅｍ．ＳｈａｎｄｏｎｇＮｏｒｍａｌ...     

A SENSITIVE PROTEIN ASSAY BY Co(II)-BIURET METHOD

ＡＳＥＮＳＩＴＩＶＥＰＲＯＴＥＩＮＡＳＳＡＹＢＹＣｏ（ＩＩ）－ＢＩＵＲＥＴＭＥＴＨＯＤ￥ＹｕｎＸｉａｎｇＣＩ；ＸｉａｏＴｉｎｇＴＡＮＧａｎｄＸｉａｏＤａＹＡＮＧ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，ＰｅｋｉｎｇＵｎｉｖｅｒｓｉｔｙ，Ｂｅｉｊｉ...     

A NEW METHOD FOR PREPARATION OF IRON（Ⅲ） PORPHYRIN OXYANION COMPLEXES－SYNTHESIS OF PERCHLORATE（PORPHYINATO） IRON（Ⅲ）

ＡＮＥＷＭＥＴＨＯＤＦＯＲＰＢＥＰＡＲＡＴＩＯＮＯＦＩＢＯＮ（Ⅲ）ＰＯＲＰＨＹＲＩＮＯＸＹＡＮＩＯＮＯＭＰＬＥＸＥＳ－ＳＹＮＴＨＥＳＩＳＯＦＰＥＲＣＨＬＯＲＡＴＥ（ＰＯＲＰＨＹＩＮＡＴＯ）ＩＲＯＮ（Ⅲ）￥ＸｉｎＨｕａＺＨＯＮＧ；ＹａｏＹｕＦＥＮＧ；Ｊ...     

MICROWAVE EFFECTS ON THE OXIDATIVE COUPLING OF MIETHANE OVER Li_2SO_4／BaCe_（0．93）La_（0．07）O_3

ＭＩＣＲＯＷＡＶＥＥＦＦＥＣＴＳＯＮＴＨＥＯＸＩＤＡＴＩＶＥＣＯＵＰＬＩＮＧＯＦＭＩＥＴＨＡＮＥＯＶＥＲＬｉ＿２ＳＯ＿４／ＢａＣｅ＿（０．９３）Ｌａ＿（０．０７）Ｏ＿３￥ＣｈａｎｇＬｉｎＣＨＥＮ；ＰｉｎＪｉｅＨＯＮＧ；ＳｈｕＳｈａｎＤＡＩ；Ｇｕａｎｇ...     

SYNTHESIS， STRUCTURE AND THERMOREANGEMENT OF TRTRA METHYLDISILANDIYL BIS（1－INDENYL） TETRACARBONYL DI－IRON

ＳＹＮＴＨＥＳＩＳ，ＳＴＲＵＣＴＵＲＥＡＮＤＴＨＥＲＭＯＲＥＡＮＧＥＭＥＮＴＯＦＴＲＴＲＡＭＥＴＨＹＬＤＩＳＩＬＡＮＤＩＹＬＢＩＳ（１－ＩＮＤＥＮＹＬ）ＴＥＴＲＡＣＡＲＢＯＮＹＬＤＩ－ＩＲＯＮ￥ＸｉｕＺｈｏｎｇＺＨＯＵ；ＢａｉＱｕａｎＷＡＮＧ；Ｓｈａ...     

Simultaneous Determination of Phytohormones in Plant Extracts using SPME and HPLC

Solid-phase microextraction followed by HPLC was used for the determination of indole-3-acetic acid (IAA), abscisic acid (ABA), indole-3-butyric acid (IBA) and 1-naphthylacetic acid (NAA) in plant samples. Parameters influencing performance, including pH, salinity, extraction time, fiber coating and temperature, were optimized. A Carbowax-coated fiber was chosen for determination due to much higher extraction efficiency compared to polyacrylate fibers. The dynamic ranges spanned over three orders of magnitude. The LOD/(LOQ) values of the target compounds in pure water were 0.149(0.497), 0.442(1.472), 0.121(0.403), 0.058(0.193) μg L⁻¹ for IAA, ABA, IBA and NAA respectively. The method was successfully applied to the analysis of xylem fluid from Musa basjoo stem obtaining recoveries of 98.85% (IAA), 94% (IBA) and 94.30% (NAA). The method was also successfully applied to the analysis of these four target compounds in the hyperaccumulating plant, Viola baoshanensis. The results matched quite well with ones obtained by solid phase extraction followed by HPLC. The method developed was superior when applied to liquid samples because matrix effects could be eliminated.     

气相色谱法分离和测定3种植物内源激素

 应用大口径毛细管气相色谱法,以正二十二烷为内标物,对植物组织中的吲哚乙酸(IAA)、脱落酸(ABA)和赤霉素(GA)等3种内源激素进行了测定。结果表明:IAA,ABA和GA的最低检测限依次为0.16,0.08和0.48mgL,相对标准偏差均小于3.0%,平均回收率为88.4%～92.2%。方法简便、灵敏、准确、重现性好。     

高效毛细管电泳法测定毛白杨雄花芽中的IAA与GA3

建立了高效毛细管电泳测定毛白杨雄花芽中生长素(IAA)和赤霉素(GA3)含量的分析方法。以甲醇为溶剂,超声提取毛白杨雄花芽中的IAA和GA3,经分离纯化后用作供试液。研究了缓冲溶液浓度、pH值、分离电压、分离温度及进样时间等因素对分离检测的影响。确定最佳测定条件为:运行缓冲液为pH 8.0的10 mmol/L硼砂和2.5 mmmol/L SDS溶液,50 mbar压力进样5 s,温度为25℃,运行电压22 kV,检测波长200 nm。最佳条件下,IAA和GA3分别在0.04～0.2 mg/L和0.2～1.00 mg/L的范围内呈良好线性,相关系数分别为0.995 2和0.999 8。2种待测物可在10 min内得到完全分离。该方法简单,分离快速,回收率高,可用于同时检测植物样品中的IAA和GA3。     

Determination of phytohormones in plant samples based on the precolumn fluorescent derivatization with 1,3,5,7-tetramethyl-8-aminozide-difluoroboradiaza-s-indacene by HPLC for routine use

Six phytohormones including indole butyric acid (IBA), naphthalene acetic acid (NAA), 2,4-dichloro-phenoxy acetic acid (2,4-D), indole-3-acetic acid (IAA), abscisic acid (ABA), and salicylic acid (SA) in crude plant extractions have been quantitated by means of high-performance liquid chromatography (HPLC) with fluorescence detection based on the precolumn derivatization using 1,3,5,7-tetramethyl-8-aminozide-difluoroboradiaza-s-indacene (BODIPY-aminozide), a fluorescent reagent synthesized in our lab recently. The optimization of derivatization conditions was carefully studied by an L(25) (5(6)) orthogonal array design (OAD) with five factors at five levels that are important influence parameters in the improvement of derivatization efficiency. The separation conditions were also studied in detail. Under the optimal conditions, the detection limits (S/N=3) of the six phytohormones were found from 0.12 to 0.75 nM. The proposed method was the first investigation of aminozide for the analysis of phytohormones and has been successfully applied to the determination of phytohormones in plant samples such as cucumber and tomato with recoveries of 94-105%.     

Diamino moiety functionalized silica nanoparticles as pseudostationary phase in capillary electrochromatography separation of plant auxins

A novel and simple method for the preparation of silica nanoparticles having surface-functionalized diamino moiety (dASNPs) was reported in our paper and characterized using scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectrometry, and thermogravimetry techniques. To test this method practically, in this contribution we describe the enhanced separation of four plant auxins - indole-3-acetic acid (IAA), indole-3-butyric acid (IBA), 2,4-dichlorophenoxyacetic acid (dCPAA), and 2-(1-naphthyl) acetic acid (NAA) - by capillary electrochromatography using diamino moiety functionalized silica nanoparticles as pseudostationary phase (PSP) in the running buffer. The effect of pH, buffer concentration, and diamino moiety functionalized silica nanoparticles concentration on the selectivity of separation was investigated. A combination of the nanoparticles and running buffer reversed the electroosmotic direction making possible the rapid and efficient separation of the auxins from the auxins migrated in the same direction with the EOF under optimum experimental conditions. A good resolution of four auxins was obtained within 5.5 min under optimum experimental conditions. The precision (RSD, n = 5) was in the range of 0.72-0.91% and 1.89-2.23% for migration time and peak area response, respectively. The detection limits were 0.48, 0.44, 0.46, and 0.42 μM for NAA, IBA, IAA, and dCPAA, respectively. Furthermore, the method was successfully tested for the determination of IAA in the grapes.     

Separation of plant hormones from biofertilizer by capillary electrophoresis using a capillary coated dynamically with polycationic polymers.

A new, simple and rapid capillary electrophoresis (CE) method, using hexadimethrine bromide (HDB) as electroosmotic flow (EOF) modifier, was developed for the identification and quantitative determination of four plant hormones, including gibberellin A3 (GA3), indole-3-acetic acid (IAA), alpha-naphthaleneacetic acid (NAA) and 4-chlorophenoxyacetic acid (4-CA). The optimum separation was achieved with 20 mM borate buffer at pH 10.00 containing 0.005% (w/v) of HDB. The applied voltage was -25 kV and the capillary temperature was kept constant at 25 degrees C. Salicylic acid was used as internal standard for quantification. The calibration dependencies exhibited good linearity within the ratios of the concentrations of standard samples and internal standard and the ratios of the peak areas of samples and internal standard. The correlation coefficients were from 0.9952 to 0.9997. The relative standard deviations of migration times and peak areas were < 1.93 and 6.84%, respectively. The effects of buffer pH, the concentration of HDB and the voltage on the resolution were studied systematically. By this method, the contents of plant hormone in biofertilizer were successfully determined within 7 min, with satisfactory repeatability and recovery.     

部分水溶性维生素胶束电动毛细管色谱行为研究

详细探讨了十二烷基硫酸钠浓度、硼砂浓度、溶液PH值、电泳电压对部分水溶性维生素胶束电动毛细管色谱行为的影响,在优化条件下,4min内完成5种水溶性维生素的分离。     

胶束电动毛细管色谱法检测红曲米中的莫纳可林K

建立了测定红曲米中莫纳可林K含量的胶束电动毛细管色谱(MEKC)方法。考察了运行缓冲液的种类、pH及其浓度、有机添加剂、十二烷基硫酸钠(SDS)的浓度和分离电压等实验条件对电泳分离效果及检测灵敏度的影响。在优化的实验条件下,以20 mmol/L硼砂(pH 10.6,含10%(体积分数)乙醇和40 mmol/L SDS)作为缓冲溶液,莫纳可林K能在23 min内实现很好的基线分离,线性范围为5.00～100.00 mg/L,线性相关系数为0.9976,检出限(以信噪比(S/N)为3计)为0.13 mg/L,加标回收率为98.5%～99.5%。精密度和稳定性试验中,峰面积和迁移时间的相对标准偏差均小于3%,表明重复性良好。该方法简便、快速、灵敏,可用于红曲米中莫纳可林K含量的测定。     

On-line coupling of pressurized capillary electrochromatography with end-column amperometric detection for analysis of estrogens

An improved technique, pressurized capillary electrochromatography (pCEC) coupling with end-column amperometric detection (AD), was developed and used for the separation and determination of estrogens. The effects of pH value, composition of mobile phase, concentration of the surfactant sodium dodecyl sulfate (SDS) and applied voltage on separation were investigated. The electrochemical oxidation of diethylstilbestrol (DES), dienestrol (DE), and hexestrol (HEX) could be reliably monitored with a carbon electrode at 0.9 V (vs. Ag/AgCl). The pCEC analyses were performed on a capillary separation column packed with 3 microm C18 particles with an acetonitrile/water (31%: 69%) mobile phase containing Tris buffer (5 mmol/L, pH 4.5) and 4 mmol/L SDS. High voltage up to 12 kV reduced the retention time dramatically and still provided a baseline resolution. In addition, supplementary pressure prevented bubble formation and provided reliability and reproducibility of the pCEC performance. The detection limits for the three estrogens ranged from 1.2 to 2.2x10(-7) mol/L, about 10 20-fold lower than those obtained with pCEC-UV detection. To evaluate the feasibility and reliability of this system, the proposed pCEC-AD method was further demonstrated with fish muscle samples spiked with estrogens.     

Analysis of three effective components in Fructus corni and its preparations by micellar electrokinetic capillary chromatography

An efficient micellar electrokinetic capillary chromatography method was developed to analyze three major active components including morroniside, loganin and gallic acid in Fructus corni and its six preparations for the first time. The factors that could affect the separation were studied, such as the pH of the buffer, concentrations of SDS, organic modifier and beta-CD, and the applied voltage. The optimum analysis conditions were 10 mmol/L NaH(2)PO(4)-5 mmol/L Na(2)B(4)O(7) (pH 6.8) buffer containing 140 mmol/L SDS, 1 mmol/L beta-CD, 5% (v/v) methanol and 12.5 kV applied voltage. The linearity between the peak-areas and the concentrations of the analytes were investigated, and they exhibit excellent linear behavior over the concentration ranges (correlation coefficients 0.9953-0.9995). In addition, the pK(a) of gallic acid was determined using capillary zone electrophoresis. The result was consistent with that reported by the literature.