高效液相色谱法鉴别染料型黑色喷墨打印字迹

目的建立液相色谱分析方法,对市售的30种不同厂家牌号（原装）染料型黑色喷墨打印字迹进行区分鉴别。方法通过选择最佳的提取条件、流动相,考察纸张、字迹形成方式等的影响,及样品及仪器的稳定性实验,确定实验条件。结果选择了最佳的反相高效液相色谱（RP-HPLC）分析方法：固定相为X-bridge Shield RP18（3.5μm,4.6×100mm）,流动相为乙腈-NH4HCO3溶液（10mmol/L）,梯度洗脱,检测波长为585nm、475nm;用该方法,根据字迹染料成分的差异将30种样品分为四大类17小类。结论该方法可以为鉴别区分不同厂家染料型黑色喷墨打印字迹提供依据。     

高效液相色谱法鉴别指甲油的种类

目的建立一种简便快速、灵敏准确的鉴别指甲油样品的方法。方法以乙腈为提取剂,在乙腈/水（80∶20）,检测波长为UV-220nm的色谱条件下,对22种不同产地、不同品牌的指甲油样品进行HPLC分析。结果依据指甲油中组分的不同,可将其分为5大类,每类中各个样品又可根据其色谱峰峰面积比的不同,进一步进行种类的鉴别。结论该方法是一种简便、快速、准确的鉴别指甲油的方法。     

全血中利多卡因的高效液相色谱法测定

本文报道反相高效液相色谱法测定全血中利多卡因浓度的方法。氟安定作为内标,全血经溶血,1N 氢氧化钠1ml 碱化后,用乙醚提取。以Zorbax ODS 为固定相,以CH_3 OH∶H_2O∶(C_2H_5) _3N(100∶45∶0. 2,pH6. 3) 为流动相,检测波长为240nm。用利多卡因为内标的峰高比定量。血中利多卡因最低检出浓度为0. 125ug/ml。线性范围是0. 0025～0. 0750mg/ml(r=0. 9999) 和0. 0250～0. 3000mg/ml(r=0. 9999) 。本法添加利多卡因1. 0、2. 5,8. 0ug 的回收率分别为101. 51±1. 51%、98. 10±2. 05%和±98. 09±3. 63%,天内变异系数分别为1. 49、1. 29和3. 70,天间变异系数为1. 78%。     

高效液相色谱法鉴别红色原子印油种类实验条件的选择

目的确定高效液相色谱法(HPLC)鉴别红色原子印油种类的实验条件。方法利用HPLC法对印油样品的提取剂、提取时间、纸张影响以及检测波长和流动相进行了测试。结果得到了样品的色谱图和定量分析数据。结论得到较佳实验条件。     

高效液相色谱法测定人血液、尿液中的2,4-D丁酯

目的建立检测血液、尿液中2,4-D丁酯的高效液相色谱分析方法。方法采用正己烷为样品萃取溶剂,色谱柱为Zorbax SB-Aq柱,流动相为V（甲醇）∶V（水）=60∶40。结果 2,4-D丁酯在血液和尿液中的线性范围分别为0.10～10.00μg/mL（r≥0.999 8）和0.08～8.00μg/mL（r≥0.999 5）,检测限分别为0.002 0μg/mL和0.001 8μg/mL,准确度为94.5%～104.5%,日内、日间精密度≤4.5%。结论本研究建立的血液、尿液中2,4-D丁酯的提取和HPLC检测方法,可应用于2,4-D丁酯中毒的快速检验和中毒死亡的法医学鉴定。     

高效液相色谱法鉴别蓝色签字笔墨水的种类

目的通过对签字笔字迹成分进行检验，达到对签字笔成分进行分离并对签字笔种类进行鉴定的目的。方法使用高效液相色谱法对蓝色签字笔字迹色痕中的色料成分进行分析，并依据分析结果对墨水的种类划分，同时考察了纸张的背景影响、最小用样量以及实验结果的重现性。结果22种蓝色签字笔样品均可以实现区分。结论本研究对实际应用有较大参考价值。     

灭多威的高效液相色谱分析

本文详细讨论了用有机溶剂从动物油脂中提取农药灭多威,用紫外分光光度法和高效液相色谱法定性定量分析灭多威的方法,得出高效液相色谱分析灭多威的最佳色谱条件及其定量标准曲线;测出用甲醇溶剂从猪油中提取灭多威的提取率为100％;测出灭多威的最小检出量为0.17μg。     

反相高效液相色谱法测定全血中青霉素类药

建立了反相高效液相色谱法测定血液中青霉素类药物。０．５ｍｌ血液中,加入甲砜霉素作为内标物,经乙腈沉淀蛋白后,上清液直接进样分析。五种青霉素类药物的线性良好,ｒ为０．９９１８～０．９９９６;相对回收率为９１．７５％～１０７．３３％;变异系数为３．５６％～９．８５％。考察了保存温度对药物分解的影响以及药物在动物血液中消除时限,排除了其它抗生素的干扰     

高效液相色谱法测定海洛因含量的不确定度评定

目的建立高效液相色谱法测定海洛因含量的不确定度评定的方法。方法结合海洛因含量测定的全部过程,假设传播系数为1,对产生不确定度的各分量因子进行分析计算与合成。结果不确定度的来源主要包含样品检测时产生的误差值、检测仪器的精密度、天平和使用的容量器皿等的不确定度。结论本评定方法得出检测的误差来自于两个平行样品检测时产生的误差值。     

高效液相色谱法检测人脊髓中的利多卡因

建立高效液相色谱法对人脊髓中利多卡因进行分析的方法 ,以扩大药 (毒 )物检测范围及检测手段 ,适应法医学鉴定及对特殊检材检验的需要。用利多卡因标准品及空白脊髓标准添加实验 ,对色谱条件、样品处理方法、回收率及方法的线性和精密度进行了系统考察。所建方法线性范围是2 0～20 0μg/ml(r=0 9999) ,最低检测限为0 2μg/ml(S/N≥3),加样回收率为82 4 %～92 7% ,该法选择性好、不受干扰。所建方法灵敏、准确、简捷 ,可用于法医学鉴定。     

人脑脊液中利多卡因的高效液相色谱分析

目的 建立人脑脊液中利多卡因的高效液相色谱(HPLC)分析方法。方法 以空白人脑脊液添加标准利多卡因进行HPLC分析,并系统考察实验中的色谱条件、样品处理方法、线性关系、精密度及回收率。结果 所建方法的线性范围是1.0～20.0μg·ml-1(r=0.9993),最低检测浓度为1.0μg·ml-1(S/N≥3),日内、日间检测的相对标准偏差≤3.0％,回收率为98.3％～102.7％。结论 所建方法定量检测人脑脊液中的利多卡,灵敏、准确、快速。     

Analysis of forensic soil samples via high-performance liquid chromatography and ion chromatography

Traditional forensic soil comparisons are performed via physical and/or chemical examinations of color, texture, and mineral content, leaving any organic- or water-soluble fractions unexamined. This study uses high-performance liquid chromatography (HPLC) and ion chromatography (IC) to assess the qualitative and quantitative variation in these fractions of soil. Soil samples (n=120) were collected over the course of 3 weeks from urban, suburban, and rural locations in and around Lansing, MI. Additional samples from six of these locations (two urban, two suburban, and two rural) were collected once a week for 10 weeks for temporal analysis. Nine additional samples, equally spaced over a 1 m(2) grid, from these same six locations were collected for spatial analyses. Qualitative and quantitative analysis of the resultant chromatograms separated the 120 samples into 10 groups by HPLC and 23 groups by IC. This study shows that using HPLC and IC to analyze the organic- and water-soluble fractions of soil can successfully discriminate samples. Quantitative analysis of the results eliminates some false inclusions by providing further differentiation of samples. The results of this study indicate that adding HPLC and IC analyses to traditional forensic soil analysis schemes can improve overall sample differentiation. The methods used in this study were also able to detect both qualitative and quantitative variations in soil over a relatively small geographic area. This demonstration of soil heterogeneity underscores the importance of the collection of a representative known sample population when assessing a forensic soil comparison. Significant temporal variation was also demonstrated over the course of 10 weeks of sampling; however, samples were found to be consistent over shorter periods of time. Baseline levels of inorganic anions were determined via IC; these levels may be useful in assessing the significance of anions detected in soil from cases involving low explosives.     

Analysis of penicillins in whole blood by reversed high-performance liquid chromatography

A reversed-HPLC method was established to determinate penicillins in whole blood. Thiamphenicol as internal standard was added to 0.5 ml blood. Proteins in blood were precipitated with acetonitrile, then the separate supernatant was directly injected onto the chromatography column. The range of five penicillins' linearities was 0.9918 to 0.9996, their range of relative recovery was 91.75% to 107.33%, their CV was 3.56% to 9.85%. Effects of different storage temperatures on the stability of analytes and interference of other antibiotics were also studied.     

Determination of bromadiolone in whole blood by high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry

A rapid, sensitive and selective high-performance liquid chromatography tandem mass spectrometric method (HPLC/MS-MS) has been developed and validated for the determination of bromadiolone in whole blood using warfarin as an internal standard (IS). Bromadiolone was extracted from the whole blood samples by liquid-liquid extraction with ethyl acetate. Multiple-reaction monitoring (MRM) was used to detect bromadiolone and IS, using precursor --> product ion combinations at m/z 527 --> 465 and 307 --> 161, respectively. The calibration curve was linear (r2=0.998) in the concentration range of 0.5-100.0 ng/mL with a lower limit of quantification of 0.5 ng/mL in whole blood. Intra- and inter-day relative standard deviations (R.S.D.s) were less than 7.5 and 11.9%, respectively. Recoveries of bromadiolone ranged from 82.1 to 85.2%. This method is found to be determined trace bromadiolone in whole blood and can be used in the diagnosis of the poisoned human beings.     

变性高效液相色谱及其在法医DNA分析中的应用

变性高效液相色谱(DHPLC)是目前检测基因突变的最佳技术平台之一。本文简要介绍了DHPLC的工作原理及主要技术特点,并对其在法医DNA分析中的应用进行综述。     

Analysis of amphetamines by supercritical fluid chromatography,high-performance liquid chromatography,gas chromatography and capillary zone electrophoresis; a preliminary comparison

A supercritical fluid chromatographic method with UV detection (SFC–UV) for the quantitative separation of phenylisothiocyanate (PITC)-derivatised amphetamines is described and compared to high-performance liquid chromatography–diode array detection (HPLC–DAD), gas chromatography–flame ionisation detection (GC–FID) and capillary zone electrophoresis–diode array detection (CZE–DAD) analyses of amphetamine and related compounds. Difficulties in the analysis of common amphetamines by SFC are discussed. Of the methods described in this paper, the SFC method offered the greatest sensitivity at 0.01–0.02 μg of drug on column. Suggestions are made for the use of combinations of these techniques for the identification of amphetamines when gas chromatography–mass spectrometry is not available.     

Determination of cocaine and its metabolites in brain tissue using high-flow solid-phase extraction columns and high-performance liquid chromatography.

A new solid-phase extraction procedure for the determination of cocaine and some of its metabolites in brain tissue, using high-flow co-polymeric sorbents is reported as a substantial improvement on our recently reported procedure. The recovery of cocaine, norcocaine and cocaethylene was excellent as was the reproducibility of the extraction. The use of high-flow sorbents allowed the easy extraction of tissue without the need for a time-consuming lipase digestion, regardless of sample viscosity or physical nature. The use of these solid-phase columns provided many advantages over the more commonly used solvent extraction, including an increase in extraction speed and efficiency, reduced operator time, reduced solvent use and disposal volumes and exceptional extract quality. The procedure was successfully applied to rabbit brains spiked with cocaine, benzoylecgonine, norcocaine and cocaethylene.     

反相高效液相色谱法测定人血浆中的吲哚美辛

建立血浆中吲哚美辛的高效液相色谱分析方法 ,扩大药 (毒 )物检测范围及手段 ,以适应法医学鉴定的特殊需要。以空白血浆标准添加吲哚美辛对样品处理方法、线性关系、回收率及精度进行考察 ,并以所建方法对健康受试者的血液浓度进行监测。方法的线性范围是 0 1～ 5 0 μg·ml-1,γ =0 9995 ,最小检出浓度为 0 0 2 μg·ml-1(S/N≥ 3)。日内、日间的方法精密度为 ( 1 1± 0 2 ) % (n =4)和 ( 2 7± 0 6 ) % (n =4) ,加样回收率为 97 5 %～10 4 2 %。所建方法准确、便捷、选择性好 ,可用于法医学鉴定及血液浓度监测     

Determination of benzodiazepines in human hair by on-line high-performance liquid chromatography using a restricted access extraction column.

A method is described for the identification of five frequently prescribed benzodiazepines (BZD) (clonazepam, diazepam, flunitrazepam, midazolam and oxazepam) in human hair samples by reversed phase HPLC, following on-line simple enrichment and clean-up on a restricted access extraction column. 50mg of powdered hair were incubated (2h at 45 degrees C) after sonication (1h) in 1 ml of the following solution (methanol:ammonia, 97.5/2.5, v/v). The aliquot was centrifuged and the methanolic phase transferred to a conical tube and evaporated under a gentle stream of nitrogen. The residue was reconstituted by adding 100 microl of a mixture of phosphate buffer (20mM, pH=2.2) and acetonitrile (94/6, v/v). A total of 80 microl were injected into the system with the column switching technique. The pre-column or clean-up column was washed with phosphate buffer pH=7.2. The drugs retained on the pre-column were then eluted in the back-flush mode and separated on a C(8) semi micro column, Lichrospher select B, 125 mm x 3 mm. The BZD were determined by a photodiode-array detector at 254 nm, using reference data (retention time and UV spectra) stored in a personal library. The method showed excellent linearity between 0.5 and 20 ng/mg of hair for clonazepam, flunitrazepam and midazolam and between 0.5 and 100 ng/mg of hair for diazepam and oxazepam. Finally, the present method has been applied to a number of forensic cases in our laboratory.