薄层色谱法分析葵花仁粕中的绿原酸

 以聚酰胺薄膜为固定相、体积分数为 36 %的乙酸溶液为流动相 ,研究建立了薄层色谱分离测定葵花仁粕中绿原酸的方法。绿原酸样品溶液上行展开 8 5cm ,其Rf 值为 0 6 1。绿原酸的检测量在 0 0 5 μg～ 0 6 μg范围内 ,其斑点的面积与绿原酸的检测量具有良好的线性关系。绿原酸的回收率为 97 5 3 % ,不同薄层板之间的RSD为2 5 7% ,最低检出限为 0 0 2 5 μg。在以体积分数为 70 %的乙醇溶液为萃取剂、搅拌振荡萃取时间为 30min的条件下 ,以该方法测定萃取液中绿原酸的含量和葵花仁粕中绿原酸的残留量 ,确定了最佳萃取次数。     

薄层扫描法测定蔗糖脂肪酸酯中的各组成酯

 建立了蔗糖脂肪酸酯中一酯～三酯的薄层分离定性及薄层扫描定量方法。以氯仿 甲醇 醋酸 水 (体积比为 80∶1 0∶8∶1 )为展开剂 ,双波长反射法锯齿扫描 ,测定波长为 530nm ,参比波长为 70 0nm ,线性范围为 4μg～60 μg ,相关系数为0 9940～ 0 9980 ,平均回收率为 96 45%～ 98 73% (RSD为 2 8%～ 3 3% ,n =3)。方法可靠 ,数据准确 ,操作简便易行 ,线性范围宽。     

高效液相色谱-蒸发光散射检测法测定合成产物中的果糖棕榈酸酯

建立了反相高效液相色谱-蒸发光散射检测（HPLC-ELSD）测定合成产物中的果糖棕榈酸单酯和果糖棕榈酸双酯的方法。HPLC-ELSD条件为：反相Prevail C18色谱柱,柱温为30 ℃,流动相为乙酸乙酯-甲醇-水（体积比为59.4∶30∶10.6）,流速为1 mL/min,ELSD漂移管温度为73.8 ℃,载气流速为2 L/min。在该色谱条件下,果糖棕榈酸单酯及果糖棕榈酸双酯在进样量为1～15 μg时,与其峰面积的线性关系良好,相关系数r2均大于0.9996。     

柱切换-荧光检测反相高效液相色谱法测定血浆中特布他林浓度

采用柱切换技术 荧光检测反相高效液相色谱法测定血浆中特布他林 (TB)浓度。使用LunaC8( 2 )和KromasilC18为分析柱 ( 1 5 0mm× 4.6mm ,5 μm)和预处理柱 ( 2 5mm× 4.6mm ,5 μm) ,流动相分别为pH 3 0 ,0 .0 3 3mol/L磷酸盐缓冲液∶甲醇∶乙腈 ( 92∶7∶1 )和水∶甲醇∶乙腈 ( 97∶2∶1 ) ,流速均为 1 .0ml/L。血浆样品经乙腈沉淀蛋白后进样 ,切换时间为 3 .2～ 4.2min。荧光检测 ,λex为 2 80nm ,λem为 3 0 9nm。以沙丁胺醇作内标 ,按内标法定量。标准曲线线性范围为 0 .8～ 3 2 μg/L ;最低定量限为 0 .8μg/L;TB和内标的保留时间分别为 8.7和 9.3min;日内RSD小于 4% ,日间RSD小于 9% ,方法回收率在 93 %～ 1 1 2 %。     

芜菁子中2-苯乙基异硫氰酸酯的分析

建立芜菁子中2-苯乙基异硫氰酸酯的定性和定量分析。采用溶剂萃取法、水蒸气蒸馏法、同时蒸馏萃取法提取芜菁子中的异硫氰酸酯。以甲苯∶乙酸乙酯(5∶2)为展开剂在高效硅胶G板上展开。采用YMCPack ODS(4. 6 mm×250 mm,5μm)为色谱柱,甲醇-水为流动相,梯度洗脱,检测波长242 nm。分离后的2-苯乙基异硫氰酸酯斑点清晰,分离效果好。溶剂萃取法提取的芜菁子中2-苯乙基异硫氰酸酯的含量最低(11. 93μg·g~(-1)),水蒸气蒸馏法提取的芜菁子中2-苯乙基异硫氰酸酯的含量最高(116. 37μg·g~(-1))。本实验的方法简便、重复性好,可为芜菁子质量控制提供基础数据。     

一种新型铂抗癌配合物HJ5的高效液相分析

 顺 二氯一氨 (4 氨基 2 ,2 ,6 ,6 四甲基哌啶 1 氧自由基 )合铂 (Ⅱ ) (简称HJ5 )是一种有研究与应用前景的新型铂抗癌配合物。建立了常规测定HJ5含量的高效液相分析方法。流动相为V(乙腈 )∶V(水 ) =10∶90的溶液 ,检测波长为 2 10nm ,柱为PhenomenexC18(15 0mm× 3 9mmi d ,10 μm) ;采用外标法测定了HJ5的线性方程、回收率和精密度。该方法能使HJ5峰与杂质峰很好的分离 ,其峰面积与检测量呈线性关系 ,最低检出限为 0 0 7μg。用 9g/L的氯化钠水溶液作溶剂 ,能有效抑制HJ5的水解 ,使其稳定时间达到 2h以上 。     

高效液相法测定芦荟胶囊中的芦荟甙

 建立了高效液相法测定芦荟胶囊中芦荟甙含量的方法。实验采用ODS柱 ,以甲醇 水 (体积比为 5 0∶5 0 )溶液为流动相 ,用紫外检测器于 2 98nm处检测。结果表明 ,芦荟甙的进样量为 0 0 2 μg～ 1 5 μg时 ,进样量与峰面积呈良好的线性关系 (r =0 9999) ;样品的加标回收率为 99 0 %～ 10 1 9% ;方法的精密度好 ,相对标准偏差(RSD)为 1 37% (n =6 )。方法快速、简便、准确 ,所测结果稳定、重现性好 ,可作为胶囊类保健食品质量检验的一个定量方法。     

高效液相色谱法测定11种雪莲花中的紫丁香甙及芦丁

 采用高效液相色谱法测定凤毛菊属植物雪莲花中的紫丁香甙和芦丁。用乙醇超声提取 ,以乙腈 (流动相A)和水 质量分数为 36 %的乙酸水溶液 (体积比为 10 0∶4) (流动相B)进行梯度洗脱。结果表明 ,紫丁香甙线性范围为0 .0 5 2 5 μg～ 1.0 5 μg ,芦丁线性范围为 0 .0 6 5 8μg～ 1.32 μg ;不同种的雪莲花植物中紫丁香甙和芦丁的含量差异较大 ,应用雪莲花药材替代品时应慎重。     

反相高效液相色谱法测定小鼠血浆及组织中的阿昔洛韦浓度

 建立了测定小鼠血浆、肝、肾、脾、肺等组织中阿昔洛韦 (ACV)浓度的高效液相色谱法。色谱柱为HypersilODS ,流动相为甲醇 水 冰醋酸 (体积比为 1∶99∶0 5 )混合溶液 ,流速为 1 5mL/min ,检测波长为 2 5 2nm。ACV血浆最低检测浓度为 2 0 μg/L ,各组织最低检测浓度为 5 0ng/g。血浆及组织匀浆中的ACV浓度在 0 1mg/L～ 4mg/L及 0 1μg/g～ 4μg/ g时线性关系良好 (r >0 99)。血浆及肝匀浆中的ACV回收率分别为 97 5 %～ 10 0 0 %和 10 0 0 %～ 10 6 0 % (n =5 )。该法精密度高 ,方便 ,快捷 。     

反相银化高效液相色谱法测定银杏叶中银杏酚酸(英文)

 建立了反相银化高效液相色谱测定银杏叶中银杏酚酸含量的分析方法。在样品的浸提液中加入少量酸性盐溶液和吸附剂后 ,用一步反萃取法净化样品 ,有机相浓缩后供HPLC分析。流动相 :V(甲醇 )∶V(体积分数为 5 %的乙酸水溶液 ) =90∶10 ,其中银离子浓度 0 0 3mol·L-1,紫外检测波长 310nm。结果表明 4种银杏酚酸之间达到基线分离 ,该方法平均回收率为97 3% ,相对标准偏差 1 6 % ,最低检测量 0 0 2 6 μg ,可有效地用于银杏叶及其提取物中银杏酚酸的定量分析。     

Kinetic of catalytic sucrose esterification in aqueous media

The process of sucrose esterification in the presence of a homogeneous catalyst was developed directing the reaction to the production of weakly substituted esters. Esterification of sucrose was processed with octanoyl chloride in a discontinuous reactor, in presence of 4-dimethylaminopyridine as catalyst. The process was operated in a time interval ranging from 0 to 80 min, at temperatures from 288 to 303 K, pH=10 and at atmospheric pressure. The following conversion levels were obtained: octanoyl chloride 11-84%, primary monoester production of 9-67%, secondary monoesters of 1.3-17%. Activation energies ranging from 158 l to 300 kJ/mol characterized the stages of the process, among them the stage of formation of the DMAP/RCOCl complex (162.43 kJ/mol). The increase in primary monoesters yield due to the temperature rise, leads to an increase in the rate of the direct reaction as well as in the speed of secondary monoester conversion to primary monoesters, quantifying a selectivity in primary isomers in the following positions sequence: 6> 1" > 6".     

气相色谱-质谱法同时测定动物内脏中的14种酞酸酯类环境激素残留

开展了动物内脏中14种酞酸酯类（PAEs）环境激素残留的气相色谱-电子轰击离子源/质谱（GC-EI/MS）的分析方法研究。优化与选择了动物内脏样品的前处理条件,动物内脏样品经正己烷/二氯甲烷（1/1,v/v）混合提取剂超声提取、Florisil硅藻土固相萃取柱净化与乙酸乙酯/正己烷（2/3,v/v）混合洗脱剂洗脱和浓缩后,以邻苯二甲酸二苯基酯（DPhP）为内标物,采用GC-EI/MS的选择离子监测方式（SIM）进行定性和定量分析。当猪肝样品的加标浓度水平为100、200、400 μg/kg时,加标回收率为：60%~110%,相对标准偏差为：0.78%~10.3%;除邻苯二甲酸二（2-甲氧基乙基）酯（DMEP）与邻苯二甲酸二（2-乙氧基乙基）酯（DEEP）的检测限（MDL）分别为3.30与2.25 μg/kg外,其余的12种PAEs的MDL ≦ 1.74 μg/kg;线性范围为50 ~ 800 μg/kg,相关系数都大于0.9994。此分析方法成功地应用于6种动物内脏中14种痕量PAEs残留的分析。     

气相色谱-串联质谱法测定土壤中的邻苯二甲酸酯

建立了土壤中6种邻苯二甲酸酯的气相色谱-串联质谱(GC-MS/MS)分析方法。土壤样品用超声提取,以二氯甲烷-丙酮(1:1, v/v)混合溶液为提取溶剂,提取液经Florisil小柱净化后,经HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)分离,利用MS/MS的多反应监测(MRM)模式进行定性和定量。结果表明本方法可对样品中的邻苯二甲酸酯进行分析,在10～1000 μg/L质量浓度范围内,线性关系良好,相关系数为0.9973～0.9976;6种邻苯二甲酸酯的相对标准偏差(RSD)不大于14.3%, 2 μg/kg和10 μg/kg两个加标水平的回收率为72.9%～106.2%; 6种目标化合物的检出限为0.1～0.5 μg/kg。该方法快速准确、背景干扰较少、分析灵敏度较高,适用于土壤样品中邻苯二甲酸酯的分析。     

Separation and determination of carbohydrates in drinks by ion chromatography with a self-regenerating suppressor and an evaporative light-scattering detector

Analysis of glucose and other carbohydrates are often performed by use of normal phase HPLC methods with acetonitrile as major eluent coupled with evaporative light-scattering detector (ELSD) or by use of anion-exchange ion chromatography (IC) methods with NaOH as eluent coupled with pulsed amperimetric electrochemical detector. In this work, a novel method for the determination of carbohydrates by IC in conjunction with a self-regenerating suppressor and an ELSD detector was investigated. Three carbohydrates (glucose, fructose, and sucrose) were separated using a KOH eluent generator to avoid the effect of carbon dioxide absorption in the alkaline eluent. Due to the use of the suppressor, non-volatile components were removed and a low salt background (K+ approximately 0.070 microg/mL) can be obtained so the suppressed eluent could directly go into an ELSD detector without obvious interference of inorganic salts. After examining the changes in retention and resolution, an optimized method was established (for IC: using 32 mM KOH as the eluent at a flow rate of 1 mL/min; for ELSD: operated at 95 degrees C, 4.0 bar nitrogen with a gas flow rate of 2.0 L/min) and the linearity, reproducibility, and the limit of detection (LOD) for the three carbohydrates were further evaluated. Regression equations revealed acceptable linearity (correlation coefficients=0.994-0.998) across the working-standard range (100-1000 microg/mL for glucose and sucrose, 150-1000 microg/mL for fructose) and LODs of glucose, fructose, and sucrose were 93, 126, and 90 microg/mL, respectively. This method has successfully been applied to the determination of the three carbohydrates in carbonated cola drinks and fruit juices. The recoveries were between 95 and 113% (n=3) for different carbohydrates.     

Quality assessment for tramadol in pharmaceutical preparations with thin layer chromatography and densitometry

Research studies have been carried out to develop a chromatographic and densitometric method suitable for identification and determination of tramadol and impurities. In addition, the stability of tramadol in solutions was investigated, including an effect of solution pH, temperature and incubation time. In the first instance the conditions for identification and quantitative determination of tramadol and impurities in pharmaceutical preparations were established. The separation was performed on silica gel-coated chromatographic plates (HPTLC) using two mobile phases: (I) chloroform-methanol-glacial acetic acid (9:2:0.1, v/v/v); (II) chloroform-toluene-ethanol (9:8:1, v/v/v). The UV densitometry was carried out at lambda = 270 nm. The developed method is of high sensitivity and low detection and determination limits ranging from 0.044 to 0.35 microg. For individual constituents the recovery ranges from 93.23 to 99.66%. The next step was to evaluate the stability of tramadol and determine a method of decomposition under various experimental conditions. It was found that tramadol decomposes in various ways in acidic and basic environments producing (1RS)-[2-(3-methoxyphenyl)cyclohex-2-enyl]-N,N-dimethylmethanamine (imp. B) and (1RS, 2RS)-2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol (imp. cis-T) or imp. cis-T, respectively.     

Rapid quantification of sucrose esters in oriental tobacco by liquid chromatography-ion trap mass spectrometry

A rapid and sensitive LC-MS/MS method was developed for the quantitative determination of sucrose esters (SEs) in Oriental tobacco samples. The sample preparation involved a 10-min sonication extraction procedure with acetone and five-fold dilution of the extract with methanol. The experiment was carried out in positive ion mode by ESI IT mass spectrometer. Because of lack of authentic standards of SEs, sucrose octa-acetate (internal standard, IS) was used as a surrogate to validate the proposed method. Matrix-matched standard calibration was used for quantification of IS in the spiked samples. Under optimized MS/MS conditions, an LOQ of 3.9 microg/g was achieved for IS, with an LOD of about 1.2 microg/g. Recoveries for IS were 95-97%. Among 19 monitored SEs, the contents of 11 SEs had RSDs lower than 13.7%. The method, with very little sample handling and good sensitivity, was applied to the rapid quantification of SEs in four Oriental tobacco samples. It appears that the sum of contents of the five SEs with MW 650, 664, and 678 Da occupied approximately 80% of the total content of SEs.     

Development of an HPLC method for the determination of salidroside in beagle dog plasma after administration of salidroside injection: application to a pharmacokinetics study

A simple RP-HPLC method was established for the determination of salidroside in dog plasma. Salidroside is one of the most active ingredients of Rhodiola L. The method had within-run precision values in the range of +/- 2.3 to +/- 9.1% (n = 5) and between-run precision in the range of +/- 3.2 to +/- 9.8%. A simple protein precipitation for salidroside extraction was processed using ACN at precipitant-to-plasma volume ratio (P-P ratio) of 3:2. The extraction recoveries of salidroside at seven concentrations were higher than 63.2%. There was a linear relationship between chromatographic area and concentration over the range of 0.83-520 microg/mL for salidroside in plasma (R = 0.9926). The LOQ (S/N = 10) of the method was 0.83 microg/mL. The method was applied in a study of the pharmacokinetics of salidroside injection in six beagle dogs. The major pharmacokinetic parameters of C(max), AUC(0-24), AUC(0-infinity), and t(1/2) of salidroside in beagle dogs after i.v. administration of a single 75 mg/kg (5 mL/kg) dose were 96.16 +/- 8.59 microg/mL, 180.3 +/- 30.6 microg h/mL, 189.3 +/- 32.1 microg h/mL, and 2.006 +/- 0.615 h, respectively.     

UV spectrophotometric determination of bioflavonoids from a semisolid pharmaceutical dosage form containing Trichilia catigua Adr. Juss and Ptychopetalum olacoides Bentham standardized extract: analytical method validation and statistical procedures

A precise, accurate, and sensitive UV spectrophotometric method was developed and validated for routine quantification of total bioflavonoids, expressed as rutin, from a topical oil-in-water pharmaceutical emulsion containing the extract of Trichilia catigua Adr. Juss and Ptychopetalum olacoides Bentham. The method was validated experimentally, and the data were treated rigorously by statistical analysis. The following analytical parameters were assessed: linearity, specificity, intra- and interrun precision measured as relative standard deviation (RSD, %), intra- and interrun accuracy (E, %), recovery (Rec., %), limit of detection (LOD, microg/mL), and limit of quantification (LOQ, microg/mL). The UV spectrophotometric method was linear (r = 0.9995) for standard rutin over the concentration range of 5.0-15.0 microg/mL with specificity for total bioflavonoids (expressed as rutin) at 361.0 nm with an absence of interferents from the complex matrix; RSD of < or = 1.79%, intrarun (E = 97.88 +/- 1.75 to 99.0 +/- 0.33%) and interrun (E = 98.38 +/- 1.12 to 100.79 +/- 1.30%) accuracy; Rec. = 98.64 +/- 0.42 to 100.74 +/- 0.41%; LOD = 0.20 microg/mL; and LOQ = 0.30 microg/mL.     

Determination of the stabilizer sucrose in a plasma-derived antithrombin process solution by hydrophilic interaction chromatography with evaporative light-scattering detection

Hydrophilic interaction chromatography (HILIC) is used for the quantitation of sucrose in the range of 10-100 micro g/mL. A poly-2-hydroxyethylaspartamide column is eluted with 25% water-75% acetonitrile, and evaporative light scattering is utilized for detection. A process sample of antithrombin (Atenativ) from Octapharma AB (Stockholm, Sweden) containing 20% sucrose is analyzed. The precision for this high-performance liquid chromatographic method is a percent relative standard deviation (%RSD) of 4, limit of detection (s/n=3) of 1 microg/mL, and mean recovery of spiked samples of 101% (RSD% of 3, n=6). Analysis time is 10 min/sample. Glucose, fructose, sodium citrate, sodium phosphate, Triton X-100, and tri-n-butyl phosphate do not interfere with the method.