Simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture by high performance liquid chromatography

A reversed phase high performance liquid chromatography （HPLC） method was established for the simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture. A Grace Apollo Cl8 column （250 mm × 4.6 mm, 5 μm） was used as the stationary phase and the mobile phase was composed of acetonitrile and aqueous phosphoric acid （0.2%, v/v）. Gradient elution was carried out at the flow rate of 1.0 mL/min and the column temperature was 30 ℃. An ultraviolet （UV） detector was used with a selected wavelength of 240 nm. Calibration curves were linear within the concentration range of 4.6-45.75 μg/mL for 12, 13-dihydroxyeuparin （r〉0.9999） and 106.9-1068.9μg/mL for glycyrrhizic acid （r〉0.9999）, respectively. Recoveries were 102.18% for 12, 13-dihydroxyeuparin and 101.17% for glycyrrhizic acid. The method developed could be applied to the simultaneous determination of 12, 13- dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture.     

单位球上小Bloch型空间之间的紧复合算子

用类似于单位圆盘D上小Bloch型空间之间紧复合算子的论证方法,得到了对所有的0〈p,q〈∞,C^n中单位球上小Bloch型空间β0^Dβ0^q之间的复合算子Cφ为紧算子的充要条件：对一切l=1,2,…,n有φl∈β0^q且 1）当0〈p〈1/2时,lim ｜z｜→1 （1-｜z｜^2）^q/（1-1φ（z）｜^2）^p｜〈Rφ（z）,φ（z）〉｜=0; 2）当p=1/2时,lim｜z｜→1（1-｜z｜^2）^q/（1-｜φ（z）｜^2）^2/1｜（1-｜φ（z）｜^2）In^22/1-｜φ（z）｜2｜Rφ（z）｜^2＋｜〈Rφ（z）〉｜^2}^1/2=0; 3）当p〉1/2时,lim｜z｜→1（1-｜z｜^2）^q/（1-｜φ（z）｜^2）^p{（1-｜φ（z）｜^2）｜Rφ（z）｜^2＋1〈Rφ（z）,φ（z）〉｜^2}^1/2=0.     

Analysis and determination of diterpenoids in unprocessed and processed Euphorbia lathyris seeds by HPLC-ESI-MS

Euphorbia lathyris （Caper spurge） is a toxic and potent Chinese materia medica （T/PCMM）. This study sought a method for identifying five diterpenoids （Euphorbia factors LI-L3, L7a, and Ls） with the spectra of UV and mass, quantifying three diterpenoids L1, L2, and L8 in crude extracts of unprocessed and processed E. lathyris seeds by liquid chromatography/ electrospray ionization mass spectrometry （LC-ESI-MS）. The analysis was achieved on an Agilent Eclipse XDB-C18 column （4.6 mm× 150mm i.d., 5 μm） with an isocratic elution with a mobile phase consisting of water and acetonitrile at a flow rate of 0.25 mL/min at column temperature of 30 ℃ and UV detection was set at 272 nm. An ESI source was used with a positive ionization mode. The calibration curve was linear in the ranges of 9.9-79 μg/mL for Euphorbia factor Lb 3.8-30.5μg/mL for Euphorbia factor L2, and 1.0-20.6 μg/mL for Euphorbia factor LB. The average recoveries （n=6） of three diterpenoids were 98.39%, 91.10% and 96.94%, respectively, with RSD of 2.5%, 2.4% and 2.1%, respectively. The contents of the three diterpenoids in processed E. lathyris seeds were 3.435, 1.367 and 0.286 mg/g, respectively, which decreased more sharply than those in unprocessed E. lathyris seeds which were 4.915, 1.944 and 0.425 mg/g, respectively. The method is simple, accurate, reliable and reproducible, and it can be applied to control the quality of unprocessed and processed E. lathyris seeds.     

指标为3的单纯Mendelsohn三元系大集

一个指标为3的Mendelsohn三元系,记为MTS（v,3）,是一个对子（X,B,其中X是一个v元集,B是X中循环三元组（区组）的集合,满足X的每一个有序对都恰包含于B中的3个区组．设（X,B是一个没有重复区组的MTS（v,3）,如果（x,y,z）∈B必有（z,y,x）B则称（X,B为单纯的,记为PMTS（v,3）．不相交PMTS（v,3）大集,记为LPMTS（v,3）,是一个集合（X,B）}i,其中每个（X,B）都是一个PMTS（v,3）,并且UiBi构成了X中所有循环三元组的一个划分．本文给出了LPMTS（v,3）的一种构造方法,得到了其存在的一个无穷类：对于v=8,14（mod18）,v≠14,存在LPMTS（v,3）．     

RP-HPLC method for the simultaneous determination of daidzein,genistein and formonetin in Solanum Lyratum Thunb

A rapid method for the simultaneous determination of daidzein, genistein and formonetin in solanum Lyratum Thunb by high performance liquid chromatography (HPLC) was developed. Separation was achieved on a Diamonsil C18 column (250 mm×4.6 mm, 5 μm) with isocratic elution, using a mobile phase of methanol-tetrahydrofuran-water (44∶3∶53, v/v). The wavelength was set at 260 nm and column was maintained at 35 ℃. The linear ranges of daidzein, genistein and formonetin were 1.0-40.0, 0.1-4.0 and 0.1-4.0 μg/mL, respectively. The average recoveries were between 98.4% and 101.3%. This method could be used for the quality control of Solanum lyratum Thunb due to its simplification, reliability, rapidity and excellent precision.     

几类高阶非齐次微分方程解的增长性

研究了一类高阶非齐次微分方程 f ()k + A k -1()z f ()k -1 +  + A0()z f = Q()z ,其中 Aj()z 为有限级整函数,Q()z 为次数小于 n 的多项式,和另一类高阶非齐次微分方程 f ()k + h k -1()z eak -1z f ()k -1 +  + h1()z ea1z f ′+( A1()z ebz + A2()z edz f = Q()z ,其中hj()z ,Ai()z 为级小于1的整函数,Q()z 为次数小于 n 的多项式,在一定条件下,得到了方程解的级的精确估计.)     

LC-ESI-MS/MS, a modified method for simultaneous quantification of isoflavonoids, flavonoids, alkaloids and saponins in a Chinese herbal preparation Gegen-Qinlian decoction

A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS) method was established to simultaneously quantitate four categories of compounds (isoflavonoids, flavonoids, alkaloids and saponins) in Gegen-Qinlian decoction (GQD). These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1% (v/v) formic acid in water (A) and 0.1% (v/v) formic acid in acetonitrile (B), and delivered at a flow rate of 0.3 mL/min. All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring (MRM) mode. Linearity, accuracy, precision, recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL. The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.     

Rapid analysis of components in Rhizoma Anemarrhenae by HPLC-DAD-MS and HPLC-DAD-TOFMS

A global quality control method based on high performance liquid chromatography (HPLC) coupled with diode array detection (DAD), single quadrupole mass spectrometry (MS) and time-of-flight mass spectrometry (TOFMS) was developed for simultaneous determination of seven major components (mangiferin, neomangiferin, timosaponin E1, timosaponin E, timosaponin BⅡ, timosaponin BⅢ, and timosaponin AⅢ) and identification of most components in extracts of Rhizoma Anemarrhenae (RA). HPLC analysis was performed on an Agilent SB-C18 column (4.6 mm×150 mm, 5 μm) by gradient elution using acetonitrile and water-acetic acid(100∶0.05, v/v) as the mobile phase. Seven major components in RA were successfully separated. This quantitative method was fully validated in respect of the following performance criteria: linearity, precision, repeatability, stability, accuracy, limits of detection (LOD) and quantification (LOQ). A formula database of known compounds in RA was established, against which, most of the reported components in this herbal extract were identified effectively based on the extract masses acquired by TOFMS. This qualitative and quantitative method was successfully used to analyze the components in 10 batches of RA samples collected from different regions in China. This global quality control method, which consisted of HPLC-DAD-MS assay of seven major components and unambiguous identification of nineteen components, is suitable for routine quantification and comprehensive quality control of RA.     

Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

Objective High performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC/MS) methods were developed for the determination of ganciclovir and its related substances. Methods A Hypersil ODS2 column (4.6mm×250mm, 5μm) was used with a mobile phase of 0.02M potassium 1.0mL/min, and UV detector set at 254nm was used for monitoring the eluents. Results The method was simple, rapid, selective and capable of separating all related substances at trace level with a detection limit of 0.04μg/mL. It has been validated with respect to accuracy, precision, linearity, and limits of detection and quantification. The linearity range was 10.2-153.0μg/mL with r=0.9998. The percentage recoveries ranged from 96.7% to 101.6%, and RSD was 1.24%-1.96% (n=5). Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir. For identification of related substances, LC/MS was used. The mainly related substances of ganciclovir active pharmaceutical ingredients (API) were determined as guanine, (1, 3-dioxolan-4-yl) methyl acetate, and diacetyl guanine.     

若干合成图的星全染色

简单图G和H的合成图是指具有顶点集V（G）×V（H）的简单图G[H],它的顶点（u,v）和另一个顶点（u,v＇）相邻当且仅当或者uu＇∈E（G）,或者“u=u’且vv’∈E（H）．文中研究了n＋1阶简单图G与m阶简单图H的合成图的星全染色,其中G为Wn。,扇Fm或星Sn．得到以下结果：（1）若△（H）=2且n≥4,m≥5,则G[H]的星全色数为（2n＋1）m;（2）若x（H）=△（H）=m-1且n,m≥4,则G[H]的星全色数为2（n＋1）m-1．     

Rapid quantification of the metabolite of valacyclovir hydrochloride in human plasma by liquid chromatography-tandem mass spectrometry

Objective To establish a rapid, sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of acyclovir (the metabolite of valacyclovir hydrochloride) in human plasma. Methods After addition of ganciclovir as internal standard (IS), plasma samples were prepared by one-step protein precipitation using acetonitrile as precipitant, followed by an isocratic elution with 0.1% formic acid 3.5μm) column. Detection was performed on a triple-quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operating in positive ion and selected reaction monitoring (SRM) mode with the precursor to product ion transitions m/z 226.2→152.1 for acyclovir and m/z 256.2→152.1 for the IS. Results The analytical results demonstrated a good linearity over the ranges from 0.005 to 4μg/mL (r=0.9999) for valacyclovir hydrochloride. The relative standard deviations (RSD) of intra-batch and inter-batch were less than 4.06% and 9.23%, respectively. The limit of detection and lower limit of quantification in human plasma were 2ng/mL and 5ng/mL, respectively. Conclusion The method was simple, sensitive, accurate and reproducible and has been successfully applied to a bioequivalence study of valacyclovir hydrochloride capsules in Chinese healthy male volunteers.     

A rapid method for the determination of dopamine in porcine muscle by pre-column derivatization and HPLC with fluorescence detection

A rapid method has been developed based on the sample preparation procedure named as QuEChERS （Quick, Easy, Cheap, Effective, Rugged and Safe）, combined with reversed-phase high performance liquid chromatography with fluorescence detector and C18 column after precolumn derivatization using o-phthalaldehyde and 2-mercaptoethanol to determine dopamine in porcine muscle. Methanol and deionized water （0.1% acetic acid, v/v） with a ratio of 60：40 was used as mobile phase. The flow rate was 0.8 mL/min and dopamine was eluted within 15 min. The linearity range was 0.003-8 μg/mL with r=0.9992. The detection limit for dopamine was 4 μg/kg and the quantification limit was 9 μg/kg. Recovery studies were carried out at 0.1, 0.5 and 1.0 mg/kg fortification levels and the average recoveries obtained ranged from 90.4% to 98.2% with relative standard deviations between 3.5% and 8.1%. The method was found to be suitable for detection of dopamine in animal product tissues at the maximum residue level.     

荒漠-绿洲过渡带斑块植被表层土壤颗粒的空间异质性

以河西走廊荒漠-绿洲过渡带为研究区域,采用土壤分析筛和地统计学的方法,对研究区典型样地斑块植被表层土壤颗粒的组成特征及其空同异质性进行了研究,结果表明：1）不同粒径范围的土壤颗粒质量含量不同,其中细砂（0.25～0.075 rmm）占总土粒质量的75.135 9％,中砂（0.5～0.25 rmm）占13.273 0％,而粗砂（d＞0.5mm）和粉砂（d＜0.075 mm）的含量相对较少,分别只占5.189 5％和6.401 6：2）不同粒径范围的土壤颗粒空间异质性不同,其中粒径1mm≥d＞0.1 mm的土壤颗粒空间异质性的99.6％～88.8％是由空间自相关因素引起的,随机因素起的作用较小,其它粒径范围的土壤颗粒空间异质性的95.1％～100％是由随机因素引起的,而空间自相关因素的作用很小;3）粒径1mm≥d＞0.1 mm的土壤颗粒含量的最优拟合理论模型为曲线模型,空间异质性尺度在24～36.3 m之间,其它粒径范围的土壤颗粒含量的最优拟合模型为线状模型或块金模型,空同异质性尺度较大,均为146.36m.研究结果为进一步探讨荒漠-绿洲过渡带土壤空同异质性与植被空同格局的关系提供依据.     

RP-HPLC method for the quantitation of β-Sitosterol in Elaeagnus Gon yanthes Benth

Objective To establish an RP-HPLC method for the determination of β-Sitosterol in Elaeagnus Gonyanthes Benth. Methods The separation was performed on a luna C8 (2) (150 mm×4.6 mm, 5μm) column with the mobile phase of methanol-water (88∶12, v/v) at a flow rate of 1.0 mL/min, the detection wavelength was set at 210 nm, and the temperature of the column was maintained at 35 ℃. Results The calibration curve of β-Sitosterol was linear over the concentration range of 0.075-0.375 mg/mL (r=0.9999) and the average recovery of β-Sitosterol was 96.30% with RSD of 3.60%(n=3). Conclusion The method is simple, rapid, and accurate, and can be used for the quality control of Elaeagnus Gonyanthes Benth.     

高效液相色谱法测定水溶液中芘的实验研究

建立表面活性剂与有机物共存体系中芘测定的高效液相色谱法.采用C18反向色谱柱(2.1mm×100mm,5μm),通过调节和控制流动相、柱温、流速等因素,得到芘的优化测试条件.结果表明:流动相选用乙腈-水(80:20,V/V),流速0.20mL·min-1,柱温25℃是最优测试条件.同时,对TX-100存在与不存在情况下芘的测试结果进行比较分析,使用OriginPro 8.6对实验数据进行线性拟合,并进行统计学t检验,结果表明:X-100存在与否对水溶液中芘的测定没有显著影响.     

应用相似理论计算碳氢化合物的热力学参数

为了计算各种化合物的热力学参数,应用相似理论,提出了用物质的"相对分子量"作为相似定数,综合了烷烃(CnH2n+2)、烯烃(CnH2n)和苯(CnH2n-6)等化合物的正常沸点Tb(压力为一个标准物理大气压时物质的沸点)与临界温度Tcr之比的实验数据,导出了这3种化合物Tb/Tcr与相对分子量之间的无量纲关系式。利用所导出的公式进行计算,其结果与实验值非常吻合,除极个别的相对误差为1%~2%外,其余绝大多数的实验值与理论计算值的相对误差均小于1%。     

图的符号控制数的下界

设G是一个图,一个函数,f.V→{-1,+1}如果∑v∈N[u]f(v)≥1对于每个点u∈V成立,则称f为图G=(V,E)的一个符号控制函数.一个图G的符号控制数定义为γs(G)=min｛∑v∈V(G)f(v)|f为图G的符号控制函数｝.该文主要给出了一个图G的符号控制教γs,(G)的若干新下限,并刻划了满足γs,(G...     

Using cell membrane chromatography and HPLC-TOF/MS method for in vivo study of active components from roots of Aconitu

An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry （CMC-TOF/MS） with a high performance liquid chromatography time-of-flight mass spectrometry （HPLC-TOF/MS） was established for in     

两类图的算术标号

对于一个（p，g）图G，如果存在一个v（G）到非负整数集N0的一个映射以称为顶点标号）满足：（1）f（u）≠f（v），其中u≠v，且u，v∈V，（c）；（2）{f（u）＋f（v）｜uv∈E（G））={k，k＋d，…，k＋（g-1）d），称图G为（k，d）-算术图。证明了图Fm．4是（d，2d）-算术图和图Fm．6是（d，3d）-算术图。     

偶图符号控制数的下界

设G=（V,E）是一个图,一个实值函数f：V→{-1,＋1}满足∑v∈N[u]f（v）≥1对一切u∈V（G）都成立,则称f为图G的一个符号控制函数。图G的符号控制数定义为γs（G）=min{∑v∈V（G）f（v）｜f为图G的符号控制函数}。研究了偶图的符号控制问题,主要给出了偶图符号控制数的两个下界。