HPLC法测定小儿氨酚黄那敏颗粒剂中对乙酰氨基酚含量

目的:用反相高效液相色谱法测小儿氨酚黄那敏颗粒中对乙酰氨基酚含量。方法:采用C18色谱柱,流动相为甲醇:0.05mol/L醋酸铵溶液(15:85),检测波长为257nm。结果:对乙酰氨基酚在6～36μg/ml浓度范围内线形关系良好,r=0.9999,平均回收率99.28%(n=5),RSD=0.62%(n=5)。结论:该方法简单、快速、准确,可以有效地控制药品质量。     

高效液相色谱测定福龙口服液中的腺苷

本文介绍了等度反相高效液相色谱(HPLC)测定福龙口服液中腺苷的方法,采用μBondapak C_(18)色谱柱,以甲醇:磷酸二氢钠(0.01mol/L)=13:87(v/v)为流动相。流速为1 mL/分,在254nm波长处检测。在0.17～10.2mg/mL测定范围内腺苷的峰面积与质量浓度的线性关系良好,相关系数为0.9997;腺苷的回收率97.18%;日内测定相对标准偏差(n=6)在1.35%～2.01%之间,隔5天测定结果基本无变化,该法已成功应用于福龙口服液中腺苷的日常测定。     

高效液相色谱法测定扑热息痛药代动力学参数

采用反相高效液相色谱法测定扑热息痛在健康人体内的药代动力学参数。Zorbax ODS色谱柱,流动相为甲醇一水一冰醋酸(20:75:5),茶碱为内标,检测波长245nm,线性范围0.5～25μg/mL,r=0.9987,回收率101.58%,日内、日间测定 RSD 均小于10%,血浆中扑热息痛最低检测浓度小于0.1μg/mL。     

反相液相色谱法测定保健食品中甘草酸

样品中的甘草酸经超声提取后用反相液相色谱法测定其含量:色谱柱为Kromasil C18柱,流动相为乙腈-0.05%磷酸溶液体积比(38∶62),波长250nm,流速1.0mL/min。甘草酸在4.388~219.4μg/mL呈良好线性关系,相关系数r为0.9999,此方法快速、简单、准确、分离度好、回收率大于95.2%。     

HPLC法测定硝酸咪唑的含量

目的:建立测定硝酸咪康唑含量的高效液相色谱(HPLC)法.方法:色谱柱为C18柱(4.6mm×100mm,5μm),流动相为甲醇-乙腈-2%乙酸铵(380:300:320),检测波长为235nm.结果:硝酸咪康唑质量浓度在0.2～1.8mg/mL范围内与峰面积呈良好的线性关系(r=0.9999).结论:HPLC法准确、...     

高效液相色谱法测定茶皂苷的含量及其血药浓度

目的:建立了高效液相色谱法对茶皂苷含量及其血药浓度的测定.方法:色谱柱为Hypersil ODS(25mm,4.6*250mm),流动相为甲醇-水(90:10),流速为0.5ml/min,检测波长为215nm.结果:茶皂苷在0.16～1.28mg/mL的浓度范围内,茶皂苷的浓度与主峰面积具有良好的线性关系,回归方程:y...     

五种磺胺类药物残留的快速测定

采用反相高效液相色谱法(RP-HPLC),同时快速测定五种磺胺类药物残留.在Waters Nova-Pak C18柱上,用紫外或PDA检测器,流速1.0 mL/min,柱温35℃,于267 nm波长处检测,流动相为5 mmol/L NaH2PO4溶液-乙腈溶液(体积比为70:30),磷酸调pH 3.0.完成整个色谱分离只须3.5 min,比原来的11 min大大减少了分离时间.     

反相液相色谱法测定保健食品中甘草酸

样品中的甘草酸经超声提取后用反相液相色谱法测定其含量色谱柱为Kromasil C18柱,流动相为乙腈-0.05%磷酸溶液体积比(3862),波长250nm,流速1.0mL/min.甘草酸在4.388～219.4 μg/mL呈良好线性关系,相关系数r为0.9999,此方法快速、简单、准确、分离度好、回收率大于95.2%.     

反相高效液相色谱法测定可乐中咖啡因的含量

建立用反相高效液相色谱法(RPLC)测定可乐中咖啡因的方法。可乐试样先用超声清洗器在40℃下超声5min,然后经前处理柱过滤,除去绝大部分有机物,最后经过0.45μm水系滤膜过滤后方可进样,通过Diomonsil C18(2)5 u色谱柱分离,以甲醇+水混合溶液为流动相进行洗脱,于286 nm波长下紫外检测。咖啡因在10～150μg/mL范围内的线性关系良好,在加标水平为60,80,100μg/mL时,被测物的回收率为96.8%～101.8%。     

五种磺胺类药物残留的快速测定

采用反相高效液相色谱法(RP-HPLC),同时快速测定五种磺胺类药物残留。在Waters Nova-Pak C18 柱上,用紫外或PDA检测器,流速1.0 mL/min,柱温35℃,于267 nm波长处检测,流动相为5 mmol/L NaH2PO4 溶液-乙腈溶液(体积比为70∶30),磷酸调pH 3.0。完成整个色谱分离只须3.5 min,比原来的11 min大大减少了分离时间。     

Adsorption of ammonium dinitramide (ADN) from aqueous solutions. 1. Adsorption on powdered activated charcoal

Investigations on the adsorption of ammonium dinitramide (NH(4)N(NO(2))(2)) (ADN) from aqueous solutions on powdered activated charcoal (PAC) were carried out in order to find out an effective and easier method of separating ADN from aqueous solutions. The effectiveness of PAC in the selective adsorption of ADN from aqueous solutions of ADN (ADN-F) and ADN in presence of sulfate (SO(4)(2-)) and nitrate (NO(3)(-)) ions (ADN-PS) was examined and compared using batch and column methods. The adsorption process follows both Langmuir and Freundlich adsorption isotherms and the isotherm parameters for the models were determined. The observed data favor the formation of monolayer adsorption. The adsorption capacities were found to be 63.3, 119, 105.3 and 82 mg of ADN per g of PAC for ADN-F (batch), ADN-PS (batch), ADN-F (column) and ADN-PS (column), respectively. Break-through curves for ADN-F and ADN-PS were obtained for the optimization of separation of ADN from aqueous solutions. Elution curves were generated for the desorption of ADN from PAC using hot water as eluent.     

高效液相色谱-二极管阵列法同时测定卷烟爆珠壁材中10种水溶性合成着色剂

该文开发一种高效液相色谱-二极管阵列检测器(HPLC-PDA)同时测定卷烟爆珠中10种合成着色剂(柠檬黄、苋菜红、胭脂红、日落黄、诱惑红、亮蓝、酸性红、赤藓红、靛蓝、喹啉黄)含量的方法。样品经热水提取后通过高效液相色谱分析,以色谱峰保留时间和紫外可见光谱进行定性。流动相采用乙腈-甲醇-乙酸铵(0.02 mol/L)水溶液,检测中使用梯度洗脱,检测波长分别为427 nm、511 nm、625 nm和529 nm,外标法定量。目标化合物在0.2-25 mg/L溶度范围内线性关系良好,相关系数均大于0.99,低中高3水平的加标回收率在82.1%-105.7%之间,相对标准偏差在1.0%-5.7%,检出限为3.1-10.8 mg/kg。该方法具有简单、快速、准确的特点,能同时检测出烟用爆珠壁材中10种水溶性着色剂。该文能够为卷烟产品开发和安全评价提供技术支撑。     

等度高效液相色谱测定大豆异黄酮中大豆甙元和金雀异黄酮

本文介绍了等度高效液相色谱(HPLC)测定大豆异黄酮中二种主要成份:大豆甙元(Daidzein)和金雀异黄酮(Genistein)的方法。采用Atlantis C18色谱柱和EasyGuard C18,保护柱;以甲醇:0·1%醋酸(pH3·11)=51·5:48·5(v/v)为流动相;检测波长λ=254nm;流速1mL/min。在测定范围内(10-200ng)峰面积与质量浓度线性关系良好。大豆甙元和金雀异黄酮的相关系数分别为0·9984,0·9997·两组份回收率为97·0—102·92%·     

离子色谱法检测含蛋白质食品中三聚氰胺

目的:建立离子色谱法检测含蛋白质食品中三聚氰胺的方法。方法:样品经冰乙酸溶液提取并沉淀蛋白,Dionex OnGuardⅡ RP样品前处理小柱除去脂肪等大分子有机物,采用Dionex IonpacCS17分离柱,3mmol/L H2SO4淋洗液等度淋洗,流速:1.2mL/min,在紫外波长240nm下检测。结果:三聚氰胺在0.5-50.0mg/L的范围内,质量浓度与色谱峰面积呈良好的线性关系(R2>0.9992),方法检出限(MDL)为0.06mg/kg,不同加标量的阴性样品加标回收率在84.8%-103.2%范围内,相对标准偏差RSD<4.0%。结论:该方法简便易行、快速,无干扰,不用有毒试剂,对环境友好,检测成本低,灵敏度高,检测结果准确度高,易于推广,适合对各种含蛋白食品中三聚氰胺的检测分析。     

高效液相色谱法测定变压器油中糠醛及相关呋喃类化合物

建立了变压器油中糠醛及呋喃类化合物(5-羟甲基糠醛、2-呋喃甲醇、糠醛、2-乙酰呋喃和5-甲基-2-呋喃)的高效液相色谱分析方法。样品经固相萃取小柱(SPE)富集后,用乙腈-水混合溶剂从柱上洗脱糠醛及呋喃类化合物。采用AgilentC18柱为固定相,乙腈-水混合溶液为流动相进行分离,在二极管列阵检测器(DAD)波长为280nm和217nm处测定。5-羟甲基糠醛、2-呋喃甲醇、糠醛、2-乙酰呋喃和5-甲基-2-呋喃等5种呋喃化合物质量浓度在0.1mg/L~5.0mg/L范围内与其峰面积呈线性关系,检出限(3S/N)分别为0.01mg/L、0.02mg/L、0.01mg/L、0.01mg/L和0.02mg/L。5种组分的平均回收率83%~96%,相对标准偏差RSD均小于3%。本方法适用于变压器油样中糠醛及呋喃类化合物5种组分的检测。     

土壤中矮壮素、缩节胺的残留对番茄酱品质的影响

采用HPLC-MS/MS技术,同时测定土壤中的矮壮素和缩节胺残留。土壤样品经缓冲溶液提取后,经Agilent ZORBAX Rx-Si(l100mm×3.0mm,1.8μm)色谱柱分离,以含浓度10mmol/L NH4Ac+0.2%HCOOH的水溶液和甲醇(60:40,V/V)为流动相进行等度洗脱,经正离子多反应监测模式测定目标化合物。结果表明:两种化合物在1.0-50.0μg/L浓度范围内线性关系良好,定量限(LOQ)矮壮素为0.8μg/L,缩节胺为0.6μg/L;加标回收率平均在97.6%-99.5%;相对标准偏差(RSD)平均在2.5%-2.9%,适用于检测土壤中矮壮素和缩节胺。     

High Performance Liquid Chromatographic Determination of Sodium Cromoglycate

A simple and precise liquid chromatographic method was developed for the estimation of sodium cromoglycate (SC) in pharmaceuticals. The drug was chroma-tographed on a reverse phase C18 column. The eluants were monitored at a wavelength of 325 nm utilizing a mixture (80:20) of solution A: 0.025 M 1-octane sulfonic acid sodium salt in acetic acid (1:100), and solution B: methanol, aceto-nitrile (3:2). Solution concentrations were measured on a weight basis to avoid the use of an internal standard. The method was statistically validated for its linearity, accuracy, precision, selectivity, limit of detection and limit of quantitation. Due to its simplicity and accuracy, the authors believe that the method can be used for routine quality control analysis. It does not require any specific sample preparation except for the use of a column guard before the analytical column and a suitable profiler attached to the syringe prior to injection.     

Extraction and isolation of triazine herbicides from water and vegetables by a double trap tandem system

The ability of a two-trap tandem system, one containing a nonspecific adsorbing material, such as graphitized carbon black (Carbopack B), and the other one filled with a sulfonic acid type silica-based cation exchanger (SCX), in extracting and isolating basic compounds from real matrices was evaluated by applying this device to the determination of triazine residues in water and vegetables. After percolation through the Carbopack column (extraction cartridge) of water samples or suitably prepared vegetable extracts, the two traps were connected in series, a methylene chloride-methanol mixture was allowed to flow along them, and triazines displaced from the extraction cartridge were selectively reabsorbed via salt formation on the strong acid exchanger column (isolation cartridge). After the column was washed, the analytes were removed from the isolation cartridge by 0.7 mL of aqueous methanol containing 70 mmol/L KCl. After the internal standard was added, the final solution was directly injected into the "high-performance" liquid chromatographic apparatus, which was operated isocratically in the reverse-phase mode with UV detection at 220 nm. The analytical recoveries of eight triazines from the two matrices considered ranged between 95% and 100%. The limits of sensitivity of this method for triazines were set at 10 ng/g of vegetable material and 10 ng/L of water by sampling 100 mL of it.     

Silica xerogel as a continuous column support for high-performance liquid chromatography

A preliminary study of the chromatographic performance and permeability of a continuous silica xerogel column under reversed-phase HPLC conditions was performed. A porous chromatographic support was synthesized inside a 0.32 mm i.d. × 13 cm fused silica tube from potassium silicate solution and derivatized with dimethyloctadecylchlorosilane. The plate height at 0.01 cm/s (0.5 μL/min), near the apparent optimum linear velocity, was about 65 μm. The column efficiencies in terms of numbers of plates per meter were 5000 and 13?000 for ethyl benzoate (k = 0.8) and naphthalene (k = 2.0), respectively, at 0.5 μL/min. The major parameter affecting column efficiency was the heterogeneous morphology of the xerogel, modifications to which are expected to improve chromatographic performance. The column provided efficiencies comparable to those reported for continuous polymeric columns but less than that previously reported for a continuous silica column. Gradient elution mode was demonstrated with a mixture of polycyclic aromatic hydrocarbons. The column was highly permeable, exhibiting a linear dependence of pressure to flow rate and a back pressure of only 632 psi at 10 μL/min when a 95% aqueous mobile phase was used.     

含ADN或TKX-50的叠氮高能固体推进剂能量特性分析

利用最小自由能法研究了叠氮类［如聚叠氮缩水甘油醚(GAP)、3,3’-双叠氮甲基氧丁烷-四氢呋喃共聚醚(PBT)、聚3-甲基-3-叠氮甲基环氧丁烷(PAMMO）］高能固体推进剂的能量特性参数,重点研究了二硝酰胺铵(ADN)和5,5’-联四唑-1,1’-二氧二羟铵(TKX-50)在不同固体填料配比下对推进剂能量特性的影响规律。结果表明:在高固含量的叠氮推进剂中,用ADN取代高氯酸铵(AP),由于燃烧产物平均相对分子量降低,推进剂比冲提高;叠氮类推进剂能量由大到小为GAP、PBT、PAMMO;TKX-50用于叠氮类高能固体推进剂中,由于体系内的负氧平衡问题,TKX-50与奥克托今(HMX)、AP或ADN间存在能量的最优配比。用TKX-50完全取代HMX时,ADN/TKX-50/Al推进剂的理论比冲为2 790.6 N?s/kg,比ADN/HMX/Al推进剂的理论比冲增加了30.7 N?s/kg。