ICP-AES法测定方铅矿中多元素的方法研究

采用电感耦合等离子体原子发射光谱法(ICP-AES)进行方铅矿中多元素同时测定.通过对方铅矿样品化学处理试验建立了HCl-NH4Cl-HNO3的溶矿体系.本体系采用基体匹配、背景系数和元素干扰系数校正及元素内标法确定了最佳综合实验测试条件.本实验建立的ICP-AES法同时测定方铅矿中镉、钴、铜、铁、铟、铅、锌7种元素的方法,本方法测量相对误差RE (n=8)为1.50%～7.50%,相对标准偏差RSD (n=8)为1.7%～5.7%.经国家一级标准物质GBW 07269分析验证可以满足方铅矿单矿物样品的分析要求.     

Evaluation of astemizole purity by HPLC

A liquid chromatographic method is described for the evaluation of Astemizole purity. The method is also applicable for the analysis of pharmaceutical dosage forms of Astemizole using indole as internal standard. Separation was achieved with a micro bondapak C(18) column and phosphate buffer (pH 6.0):acetonitrile (50:50 v/v) as eluent, at a flow rate of 1.5 ml/min with UV detection at 280 nm. The method is suitable for estimating the possible impurities if any present in Astemizole up to 0.05% for 1a and 0.25% for 1b. The method is simple, rapid and accurate for the analysis of Astemizole.     

Method development and validation for zotarolimus concentration determination in stented swine arteries by liquid chromatography/tandem mass spectrometry detection

Drug-eluting stents have attracted significant attention in the medical community and pharmaceutical industry due to their proven success in significantly reducing restenosis. Abbott Laboratories is developing a drug-eluting stent coated with zotarolimus and swine was recently used as an animal model for the pre-clinical study of stent implantation. In this article, we present a detailed experimental design and results for the validation and sample analysis of zotarolimus drug concentration in stented swine artery samples. Introduction of tissue quality control (QC) samples allows evaluation of the entire analytical process as well as the stability of the drug in both original tissue and homogenized tissue samples. In addition, a novel approach using 100% swine blood as the homogenization solution was developed for the consistency of the liquid-liquid extraction recovery and stability of the zotarolimus in tissue homogenates. Standards were prepared by spiking zotarolimus working solution in swine blood and tissue QC samples were used along with the artery samples during the sample analysis. The linear dynamic range of blood standard samples is from 0.61 to 333.20 ng/mL to accommodate the predicted artery homogenate concentrations. Overall tissue QC %CV during the method validation was from 4.4% to 8.6%. The overall %bias of tissue QC samples during the method validation was from -7.3% to 16.6%. The method was successfully applied for the analysis of swine artery samples. A similar approach for method validation and sample analysis has been successfully applied for the analysis of swine myocardium, kidney and liver tissue samples.     

电感耦合等离子体发射光谱法(ICP-AES)测定螯合肥中的螯合铁含量

选用HCl(2%)处理螯合铁样品,建立了电感耦合等离子体原子发射光谱法(ICP-AES)快速测定螯合铁含量的方法,实验确定了最佳测定条件,采用标准曲线法为定量依据,得出样品的相对标准偏差(RSD)为0.42%(n=6),加标回收率为98.48%~99.43%。建立的方法处理样品简单、快速,测定结果准确可靠,令人满意。     

A multiresidue method for the determination of 109 pesticides in rice using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas chromatography/mass spectrometry with temperature control and vacuum concentration

A rapid, specific and sensitive multiresidue method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas chromatography with mass spectrometric detection by selected ion monitoring (GC/MS-SIM) has been developed for the routine analysis of 109 pesticides in rice. The method uses one quantification ion and two identification ions. Temperature control during sample preparation helps improve the recovery of thermally labile pesticides such as captan. The method was validated by the analysis of samples spiked at 0.025-0.150 mg/kg in rice matrix. The recoveries of all pesticides were between 80% and 115% with a relative standard deviation of less than 15%. The limit of quantitation (LOQ) for most compounds met the maximum residue limits (MRLs) for pesticides in rice in Korea.     

Simultaneous determination of antimony and chlorine in synthetic rubbers by 14 MeV neutron activation analysis

A nondestructive method for the analysis of Sb and Cl in synthetic rubbers by 14 MeV neutron activation analysis has been developed and evaluated by comparisons with microanalytical and thermal neutron activation analysis results. The method is most precise when a rubber with known amounts of Sb and Cl is used as a standard. Samples containing 0.07 to 2.5 wt.% Sb and 2.5 to 15.9 wt.% Cl have been analyzed and precision for the method is 10% or better. Antimony and Cl detection limits are 0.02 and 0.5 wt.% respectively. Agreement among the three methods is excellent; the thermal activation analysis method is more precise and simpler to apply if only Sb needs to be determined in a sample. This work was supported by the U.S. Department of Energy (DOE) under Contract DE-AC04-76-DP00789. A U.S. DOE facility.     

肌酐纯度标准物质的定值方法及其不确定度评定研究

通过定性及定量分析,研究了肌酐纯度标准物质的定值方法,并进行了定值分析的不确定度评定。首先使用三重四极杆质谱仪及核磁共振谱仪(氢谱)对肌酐样品进行定性分析,然后采用质量平衡法(包括液相色谱法、水分、灰分、挥发性物质和无机元素分析)与定量核磁共振法共同对肌酐纯度标准物质进行准确定值,最后对定值结果进行不确定度评定。肌酐的定值结果为99.7%,扩展不确定度为0.4%。该研究对于实际检测中肌酐的准确测定及临床上相关疾病的正确诊断治疗具有重要意义,且经过定值的肌酐纯品还可做定量核磁共振法的定量内标使用。定量分析后的肌酐经过均匀性检验和稳定性考察后可申报为国家标准物质。     

Selective extraction and analysis of pioglitazone in cow plasma using a molecularly imprinted polymer combined with ESI ion mobility spectrometry

A method based on ESI ion mobility spectrometry as a detection technique after treatment with a molecularly imprinted polymer is described for the analysis of pioglitazone. In addition to the molecularly imprinted polymer separation methodology, the positive ion mobility spectrum and the reduced mobility values for pioglitazone are reported for the first time. The method was exhaustively validated in terms of sensitivity, imprinting factor, enrichment factor, and sorption capacity. A linear dynamic range of 0.10–20.00 μg/mL and an RSD below 6% were obtained for the analysis of this compound. The average recovery for the analysis of spiked samples was calculated to be about 91%. The method was also used to determine pioglitazone in cow plasma, and the results were compared with those obtained using HPLC. The satisfactory results evidence a convenient method for the analysis of the target compound in real samples without using any additional derivatization methods.     

Collaborative study of the determination of cloxacillin by column liquid chromatography

A previously published column liquid chromatographic method proposed for the analysis of cloxacillin preparations was subjected to an interlaboratory collaborative study. The method is rigorously defined in terms of performance requirements, yet allows a degree of flexibility to the individual analyst. Eight participating laboratories submitted results for the analysis of three samples in duplicate. The data from one laboratory were rejected because they failed to meet the prescribed performance criteria. Estimates for the repeatability and reproducibility of the method, expressed as relative standard deviations of the results of the analysis of cloxacillin preparations, were found to be less than 0.65% and 1.33%, respectively.     

人参中有机磷农残的基质固相分散-HPLC同时快速分析

建立了基质固相分散-高效液相色谱法(MSPD-HPLC)对中药材人参中的三种有机磷农药甲胺磷、甲基对硫磷和乙基对硫磷残留量进行快速分析:. 将HPLC法应用于有机磷农药残留量的检测, 分别采用中性Al2O3和体积比为8%的乙酸乙酯-正己烷作为MSPD的分散剂和洗脱剂, 对分析方法的质量控制问题进行了详细讨论, 并对不同种类的人参中药材进行了准确的定性定量分析. 该方法的线性范围为0.20～10.00 mg•L－1, 相关系数(R)大于0.99815, 相对标准偏差(RSD)均小于11.54%, 检测限(LOD)低于0.017 mg•L－1, 样品的加标回收率为87.29%～92.43%. 其线性范围、相关系数、准确度、精密度和LOD等指标均满足有机磷农残分析的要求.     

Hydrocarbon group type analysis of petroleum heavy fractions using the TLC-FID technique

Hydrocarbon group type analysis is important in all conversion processes and in preparation of feed for these conversion processes so as to learn the selectivity of the different type of catalysts for product yield and quality. The use of the Mark 5 Iatroscan detector and the method reported here allowed for a rapid and quantitative hydrocarbon group type analysis of petroleum residues without prior separation of asphaltenes. SARA type analyses of petroleum residues have been performed by a three stage development using n-hexane, toluene and DCM (95%):MeOH (5%). The standard deviation and coefficient of variation in repeated measurements by this method were as low as 0.65 wt% or less and 3.5 wt% or less, respectively. The time required for analysis of 10 samples could be as short as 90 min.     

火焰原子荧光光谱法测定矿石样品中的银

为满足矿产资源领域地质找矿的检测工作需要,寻找一种操作便捷、重现性好、检出限低的检测方法,进行银元素的定量分析测试。通过对样品取样重量、复溶盐酸用量等参数进行条件优化试验,选出最优前期处理条件;对火焰原子荧光光谱仪进行条件试验,针对灯电流、燃气气流量等关键参数进行单一变量试验,最终确立了仪器最佳测试条件;测试方法精密度为精密度为1.80%～4.52%,准确度为0.46%～1.82%,检出限为0.4g/t。本方法具有稳定性好,灵敏度高,分析效率快等特点,适合在样品量多、精度要求高的实验室间推广。     

X射线荧光光谱法同时测定矿石中铀和钍

建立了X射线荧光光谱法测定矿石样品中铀、钍含量的快速分析方法。采用高压粉末制样法,对不同含量的放射性样品的压片压力、粒径、含水率、用量等处理条件到进行单因素实验。在400 MPa压力下压制,克服了低压制样的弊端,制备的样片表面光滑、致密,大幅改善了制样重现性,有效地减少了部分基体效应,铀校准曲线的标准偏差从0.053%降到0.0071%,钍校准曲线的标准偏差从0.062%降到0.0057%。经国家一级标准物质验证,表明方法准确、可靠,能满足样品中铀、钍含量日常分析要求。     

Rapid determination of fosetyl-aluminium in commercial pesticide formulations by high-performance liquid chromatography

An isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method with diode array detection (DAD) was developed for the determination of aluminium tris(ethyl phosphonate) (fosetyl-aluminium, fosetyl-Al) in plant-protection products. The method involves extraction of the active ingredient by sonication of the sample with water and direct measurement by RPHPLC. The isocratic RP-HPLC method for the analysis of fosetyl-Al thus developed was then validated for specificity, linearity, precision, and accuracy. The chromatographic peak confirmation was performed by LC-MS using electron spray ionisation in the negative-ion mode. The repeatability of the method, expressed as relative standard deviation (RSD, %), was found to be 0.5 % and the limit of detection was 0.035 mg mL^?1. The average recoveries of the three fortification levels varied from 96.7 % to 100.6 % and the RSDs ranged between 2.6 % and 6.3 %. The precision of the method was also considered to be acceptable as the experimental repeatability relative standard deviation (RSD_r) was lower than the RSD_r, calculated using the Horwitz equation. The method is rapid, simple, accurate, cost-effective, and provides a new and reliable means for the analysis of fosetyl-Al in formulated products.     

溶液聚合过程中共聚物粘均分子量的快速测定

丙烯腈;衣康酸;溶液聚合过程中共聚物粘均分子量的快速测定     

米糠中阿魏酸的提取及荧光分光光度法检测

确定了新鲜米糠中阿魏酸的最佳提取工艺。用高效液相色谱法对提取产品作定性检测,用荧光分光光度法对提取产品作定量检测。阿魏酸在0.2~2.2μg/mL浓度范围内呈良好的线性关系,相关系数为0.99958,平均回收率为99.0%。此法具有准确、简便、快速、灵敏等优点。     

Liquid chromatography-mass spectrometry-based quantification of steroidal glycoalkaloids from Solanum xanthocarpum and effect of different extraction methods on their content

A new liquid chromatography-mass spectrometry (LC-MS)-based method coupled with pressurized liquid extraction (PLE) as an efficient sample preparation technique has been developed for the quantification and fingerprint analysis of Solanum xanthocarpum. Optimum separations of the samples were achieved on a Waters MSC-18 XTerra column, using 0.5% (v/v) formic acid in water (A) and acetonitrile (ACN):2-propanol:formic acid (94.5:5:0.5, v/v/v) (B) as mobile phase. The separation was carried out using linear gradient elution with a flow rate of 1.0mL/min. The gradient was: 0min, 20% B; 14min, 30% B; 20min, 30% B; 27min, 60% B and the column was re-equilibrated to the initial condition (20% B) for 10min prior to next injection. The steroidal glycoalkaloids (SGAs) which are the major active constituents were isolated as pure compounds from the crude methanolic extract of S. xanthocarpum by preparative LC-MS and after characterization were used as external standards for the development and validation of the method. Extracts prepared by conventional Soxhlet extraction, PLE and ultrasonication were used for analysis. The method was validated for repeatability, precision (intra- and inter-day variation), accuracy (recovery) and sensitivity (limit of detection and limit of quantitation). The purpose of the work was to develop a validated method, which can be used for the quantification of SGAs in commercialized S. xanthocarpum products and the fingerprint analysis for their routine quality control.     

Hydrocarbon group type analysis of petroleum heavy fractions using the TLC-FID technique

Hydrocarbon group type analysis is important in all conversion processes and in preparation of feed for these conversion processes so as to learn the selectivity of the different type of catalysts for product yield and quality. The use of the Mark 5 Iatroscan detector and the method reported here allowed for a rapid and quantitative hydrocarbon group type analysis of petroleum residues without prior separation of asphaltenes. SARA type analyses of petroleum residues have been performed by a three stage development using n-hexane, toluene and DCM (95%):MeOH (5%). The standard deviation and coefficient of variation in repeated measurements by this method were as low as 0.65 wt% or less and 3.5 wt% or less, respectively. The time required for analysis of 10 samples could be as short as 90 min. Received: 20 May 1997 / Revised: 12 August 1997 / Accepted: 16 August 1997     

Optimization strategy and validation of one chromatographic method as approach to determine the phenolic compounds from different sources

We have designed a novel working strategy to optimize a unique chromatographic method consisting of diode array detection for the analysis of the most representative phenolic compounds from different food sources. The simultaneous inclusion of standard phenolic compounds, phenolic compounds isolated from food sources and representative real extracts as an ultimate test in analysis has allowed to establish, for the first time, a unique liquid gradient to serve as an excellent medium for the investigation of phenolics in samples from different food sources. Under the optimized conditions, 21 commercially available phenolic compounds and 25 commercially unavailable phenolic structures were analyzed in less than 30 min. The chromatographic method was designed as an alternative for the provisional identification of these compounds before their full characterization. The optimized chromatographic method was carefully validated for precision and accuracy. A high reproducibility in the retention time (<2%), peak area and calibration slope (<5%) as well as recoveries higher than 95% were obtained in all cases. Consequently, the currently described method was successfully employed to study the phenolic compounds in the most representative food samples.