胶束液相色谱法在体内毒物分析中的应用

胶束液相色谱法是采用高于临界胶束浓度的表面活性剂溶液作为流动相的反相液相色谱方法。本文概述了胶束液相色谱法的基本原理和在理化分析方面的优势,介绍了其在毒品、巴比妥类镇静催眠药、苯二氮卓艹类催眠镇定药检验等方面的实际应用,认为胶束液相色谱法具有选择性高、适用范围广、生物样品处理简便等优点,可成为毒物分析的一种方法。     

GC-MS/MS测定血液中巴比妥类安眠药物

建立GC-MS/MS测定血液中巴比妥类安眠药物的分析方法。方法通过固相萃取提取并富集血液样品中常见巴比妥类安眠药物,采用离子阱二级质谱定性并定量检测其含量,并优化萃取溶液pH值与气相色谱/二级质谱联用分析条件,对巴比妥类安眠药物进行定量分析。结果巴比妥类安眠药物检出限为0.04μg/mL～0.10μg/mL,回收率为80.3%～92.6%。结论该方法高效、简单,灵敏度高,可用于血液中巴比妥类安眠药物同时定性定量检测。     

生物检材中巴比妥类药物固相萃取及分析方法

目的建立生物检材中巴比妥类药物的提取净化和定性定量分析方法；方法应用固相萃取法提取生物检材中巴比妥类药物，比较了巴比妥类药物固相萃取的最佳pH值、固相吸附柱等提取条件；结果确定了巴比妥类药物的GC／NPD线性范围和GC／MS检出限；结论该方法实用，提取率高，杂质干扰少，为实际案件中巴比妥类药物的提取净化和定性定量分析提供了方法和依据。     

胶束液相色谱法在生物体液药物检测中的应用

胶束液相色谱法是一种以表面活性剂组成的胶束水溶液为流动相的色谱方法。胶束流动相具有毒性小、成本低、选择性好的特点,特别是在生物体液分析中能够溶解蛋白,可将血清或尿样品直接注入色谱进行分析。省去了传统液相色谱分析前样品的提取和净化步骤。使用紫外和荧光检测器灵敏度可达每毫升μ～ng。经与酶联免疫法(EMIT)对同一样品的检测比较,所得结果一致,在生化、临床及刑事毒物分析中具有广泛的应用前景。     

超高效液相色谱检测黄樟素方法研究

本文建立了检测黄樟素的超高效液相色谱定量分析方法。将黄樟素样本以甲醇稀释,1500 r/min振荡10 min或超声3 min,以0.22μm滤膜过滤后供仪器分析,对流动相梯度程序进行了考察和优化。采用岛津ODS-SP型(250mm×4.6mm,5μm)色谱柱,以高纯水(A)-乙腈(B)体系作为流动相,梯度程序为60%B(0.01min)~66.5%B(13 min)~95%B(13.01 min)~95%B(20 min),流速1 mL/min,柱温40℃,进样量5μL,主定量波长210 nm,辅定量波长235 nm。实验结果表明,随着有机相初始浓度的升高,黄樟素色谱峰的理论塔板数减小、峰高增加、保留时间缩短;随着梯度陡度的增加,黄樟素色谱峰的理论塔板数和峰高均增加、保留时间缩短。经过方法优化,所测黄樟素样品色谱行为良好,在2~200μg/mL范围内线性良好,外标工作曲线为Y=1833.39X+5675.32,相关系数高于0.9999。以信噪比S/N>3计算,检测限为0.1μg/mL。日内精密度≤1.26%,日间精密度≤2.08%。加标回收率在98.21%~102.18%之间,RSD为0.35%~0.96%。在室温放置96h、-20℃放置15 d以及在室温和-20℃反复冻融3次的条件下均可保持稳定。该方法快速、简便、高效、可靠。     

液质联用仪自动筛选常见安眠镇静药的应用研究

目的建立快速、灵敏的常见安眠镇静药物的液质联用仪的定性筛选方法。方法采用ZORBAX sb-aq,150mm×2.1mm×3.5μm(带预柱)色谱柱;柱温:30℃;流动相:甲酸(0.1%)甲醇和甲酸(0.1%)水溶液梯度条件;流速:0.4mL/min;通过电喷雾电离,自动三级扫描质谱。结果通过软件自动处理数据,建立了57种常见安眠镇静药的质谱谱库和保留时间参数谱库。结论建立的常见安眠药谱库和分析方法具有快速、灵敏、准确的优点,不易造成漏检,并且用于实际案件检验。     

毛细管气相色谱分析巴比妥类安眠药

气相色谱技术是当今毒物分析工作中应用最广泛的手段之一。对生物样品中巴比妥类药物的检测,在以往文献报道中多采用填充柱色谱技术。由于巴比妥类药物是极性有机化合物,在气相色谱分析中常出现拖尾现象,有些学者又提出在上机分析前或进样后将巴比妥类药物转变成非极性的衍生物。但这样的前处理工作繁杂,检测重现性较差,难以适应法医毒物分析工作     

合成大麻素JWH-122的高效液相色谱分析方法研究

目的研究被我国《非药用类麻醉药品和精神药品列管办法》列入管制的合成大麻素JWH-122的高效液相色谱分析方法。方法以甲醇-去离子水(50%-50%)为流动相进行梯度洗脱,考查有机相初始浓度、梯度陡度、柱温、流速等色谱条件及检测波长,确定最优实验条件,在优化条件下对线性范围及专属性进行实验,通过实际样本检测对所建方法进行验证。结果紫外光谱检测波长221nm、有机相初始浓度为70%、梯度陡度为0.5%/min、流速1.2ml/min、柱温30℃条件下JWH-122在0.002mg/ml-0.1mg/ml范围内线性良好,检出限(S/N≥3)为0.1μg/ml;实际样本检测表明,优化条件下JWH-122能与样本中其它组分很好分离。结论该方法具有快速、灵敏、准确、分离效果好的优点,适用于新型香料毒品中合成大麻素JWH-122的分析检测。     

用衍生化气相色谱法分析血液中巴比妥类安眠药

本文对衍生化气相色谱法检测人体液中巴比妥类安眠药进行了综述,列举了7种不同类型的衍生化反应,重点介绍了甲基化法的应用及其具体操作,是当今临床及法庭科学分析中较为先进、灵敏的检测技术。     

一些常见药物在ODS柱上的分离

应用高效液相色谱技术,进行药物的分离、分析已有很多报导。为了在尽可能简便的条件下.较为有效地进行一些药物,主要是弱极性结构药物的初步判断,我们采用 ODS 柱做了些探索。对于一些常见药物,如巴比妥类、安定类、解热镇痛类及某些抗菌素类药物均能观察到较为满意的分离效果。     

反相高效液相色谱分离抗精神失常药物

作者采用反相高效液相色谱法对氯丙嗪、三氟拉嗪、异丙嗪、奋乃静、氟奋乃静、氯氮平、氟哌啶醇、安泰乐,多虑平等九种常见抗精神失常药物进行分离。并对色谱条件流动相中甲醇比例,二乙胺浓度,pH值及柱温对药物保留时间的影响进行考察,选择出一种能良好分离九种药物的色谱系统,对这类药物中毒时鉴别药物品种具有实用意义。     

高效液相色谱法相对保留时间和峰高比在毒物筛选中的应用

本文用高效液相色谱法相对保留时间、２３０ｎｍ和２５０ｎｍ两个紫外检测的峰高比、荧光和２５０ｎｍ紫外检测的峰高比三个指标相结合对毒物进行筛选，３７种毒物区分率由单用保留时间区分的２４．３％提高到９４．６％，文中还考察了各种因素对相对保留时间和峰高比的影响。     

离子交换柱法萃取血样中4种巴比妥类药物

目的建立血样中4种常见巴比妥类药物的固相萃取方法。方法采用Oasis MAX固相萃取柱对样品进行预处理,以2%氨水淋洗2,%甲酸-甲醇洗脱,GC/NPD定量检验,GC/MS定性检验。结果血样中4种常见巴比妥类药物平均萃取回收率达80%以上,以信噪比10/1计,最小定量限为1～2μg/mL,以信噪比3/1计,检出限为0.5～1μg/mL,在1～50μg/mL范围内,线性相关系数均在0.99以上。结论本文固相萃取方法检出限低,回收率高,选择性强,可应用于血样中4种常见巴比妥类药物的检测。     

Achiral and chiral quantification of methamphetamine and amphetamine in human urine by semi-micro column high-performance liquid chromatography and fluorescence detection

In this paper, miniaturized achiral and chiral high-performance liquid chromatographic procedures for the determination of methamphetamine and amphetamine in human urine are described. After a simple pretreatment of human urine (i.e., 10 microL of urine or diluted urine were acidified and dried-up under N2 at room temperature) and fluorescence derivatization with 4-(4,5-diphenyl-1H-imidazol-2-yl)-benzoyl chloride under mild conditions (pH 9.0, 10 min at room temperature), the derivatives were isocratically separated on a semi-micro ODS column with Tris-HCl buffer (0.1 M, pH 7.0): acetonitrile (45 + 55 v/v) at a flow rate of 0.2 mL/min or their enantiomers were separated on a semi-micro OD-RH column with sodium hexafluorophosphate (0.3 M aq.): acetonitrile (44 + 56 v/v) at a flow rate of 0.1 mL/min as the mobile phase. Wide-ranged calibration curves were obtained with detection limits for the achiral and chiral analyses in the atto and femtomol levels, respectively, per injected volume. Satisfactory within- and between-day reproducibility data were obtained with both the methods with the highest relative standard deviation being 9.6%. The methods were applied to the determination of methamphetamine and amphetamine in human urine samples and the concentrations determined by the two methods were well correlated (r = 0.994).     

生物检材中芬太尼和舒芬太尼的HPLC-MS/MS分析

目的建立血、肝组织中芬太尼和舒芬太尼的HPLC-MS/MS分析方法。方法采用Oasis（MCX固相萃取柱进行提取,以XTerraTMRP18柱（2.1mm×100mm,3.5μm）色谱柱分离,以乙腈∶5mmol/L醋酸铵水溶液（氨水调pH=9.5）（65∶35）为流动相,流速为0.2mL/min。结果血及肝组织添加样品的线性范围为10ng/mL～500ng/mL,最小检出限为0.1ng/mL。结论本方法准确、快速,可用于生物检材血、肝组织中芬太尼和舒芬太尼的定性定量分析。     

高效液相色谱法测定小鼠血清中可卡因的含量

目的 建立一种测定血清中可卡因含量的高效液相色谱方法。方法 以0.04mol/L磷酸盐缓冲液(含有0.26 mmol/L四丁基胺盐,pH3.2)-乙腈(83:17)为流动相,血清样品采用2％异戊醇正己烷-0.1 mol/L HCl液液反萃取法处理,用Kromasil C18色谱柱分析血清中可卡因的含量。紫外检测波长为235nm。结果可卡因的最小检出浓度为25ng/ml,回收率71％。结论所建方法测定血清中可卡因含量灵敏度高,简便易行。     

Development and validation of a sensitive UPLC-MS/MS method for the analysis of narcotic analgesics in urine and whole blood in forensic context

Narcotic analgesics are widely (ab) used and sometimes only occur in low concentrations in biological samples. Therefore, a highly sensitive liquid chromatography tandem mass spectrometry method was developed for simultaneous analysis of 9 narcotic analgesics and metabolites (buprenorphine, O-desmethyltramadol, fentanyl, norbuprenorphine, norfentanyl, pethidine, piritramide, tilidine and tramadol) in urine and whole blood. Sample preparation was performed on a mixed-mode cation exchange solid phase extraction cartridge with an additional alkaline wash step to decrease matrix effects and thus increase sensitivity. Ionization with electrospray ionization was found to be more efficient than atmospheric pressure chemical ionization. The use of a mobile phase of high pH resulted in higher electrospray ionization signals than the conventional low pH mobile phases. In the final method, gradient elution with 10mM ammonium bicarbonate (pH 9) and methanol was performed on a small particle column (Acquity C18, 1.7 μm, 2.1 mm × 50 mm). Selectivity, matrix effects, recovery, linearity, sensitivity, precision, accuracy and stability were validated in urine and whole blood. All parameters were successfully evaluated and the method showed very high sensitivity, which was the major aim of this study. The applicability of the method was demonstrated by analysis of several forensic cases involving narcotic analgesics.     

HPLC simultaneous determination of glycerol and mannitol in human tissues for forensic analysis

A method for simultaneous determination of glycerol and mannitol in various human tissues was devised and for this we used high-performance liquid chromatography (HPLC). Specimens were homogenized in a mixture of chloroform and methanol, phosphate buffer (pH 7.0) and pentaerythritol (IS) solution. After centrifugation, an aliquot of the aqueous layer was evaporated to dryness and derivatized with p-nitrobenzoyl chloride at 50 degrees C for 1h, then applied to HPLC with analytical conditions of: column, CAPCELL PAK C18 MG (250 mm x 3.0 mm i.d., 5 microm, Shiseido Co. Ltd., Tokyo, Japan); column temperature, 1-2 degrees C; mobile phase, 75% acetonitrile-distilled water containing 0.05% trifluoroacetic acid, 0.05% heptafluoro-n-butyric acid and 0.1% triethylamine; flow rate, 0.5 ml/min; wavelength, 260 nm. Calibration curves for both substances were linear in concentration ranges from 1 to 500 microg/0.1g and correlation coefficients exceeded 0.99. The relative standard deviation (R.S.D.) of the method was evaluated at concentrations of 10 and 100 microg/0.1g, and ranged from 0.84 to 10.6%. Using this method, we determined the regional distribution levels of glycerol and mannitol in various tissues from an autopsied brain dead man.     

柱切换HPLC法分析尿中吗啡和O^6—单乙酰吗啡的研究

目的建立用柱切换HPLC技术分析尿中吗啡和06-单乙酰吗啡的方法.方法尿样用硼砂缓冲液(pH9.2)稀释后进入预处理柱(YWG-C18,33mm×5.0mm,10μm),用H2O洗去杂质,再用CH3OHH2O(6040)将被分析组分洗脱进入分析柱(Lichrospher(R)100CN,125mm×4.0mm,5μm),分析流动相为CH3OH磷酸盐缓冲液(pH6.86)=2278.紫外检测器波长为286nm.结果尿中吗啡和06--单乙酰吗啡的线性范围分别为50～1 600n/ml和100～1 600n/ml.吗啡和O6--单乙酰吗啡的精密度均小于4%.吗啡和O6-单乙酰吗啡的检测限均为40n/ml.结论用CSHPLC测定尿中吗啡和O6-单乙酰吗啡,方法准确、灵敏、快速、简便.