家兔血清、尿中甲基苯丙胺及其代谢产物苯丙胺的气相色谱/质谱分析

目的:建立血清、尿中甲基苯丙胺(MA)及其主要活性代谢产物苯丙胺(AP)的气相色谱/质谱(GC/MS)定性定量分析方法,探讨样品稳定性和家兔血、尿中AP和MA的比值关系。方法:样品中加入内标物丙基解痉素(SKF525A)后碱化,乙醚萃取,三氟醋酸酐衍生化,GC/MS法分析甲基苯丙胺和苯丙胺。结果:血清和尿中甲基苯丙胺与苯丙胺的线性范围分别为0.01~5.0mg.L-1和0.1~50.0mg.L-1;最低检出限为0.005mg.L-1(S/N≥3);提取回收率均大于74.3%;方法回收率为95.50%~103.16%;日内及日间RSD均小于10%。18h内苯丙胺与甲基苯丙胺在血、尿中比值分别为0.16~1.5和0.021~0.079。血清样品在室温和冷冻条件下存放24h甲基苯丙胺、苯丙胺的相对误差为5.3%~6.1%。结论:甲基苯丙胺中毒血清样品在室温和冷冻条件下稳定,建立的GC/MS分析方法同时测定血清和尿液中甲基苯丙胺及其主要代谢产物苯丙胺,方法简便、灵敏、重复性好,适用于甲基苯丙胺中毒与滥用案例的快速鉴定。     

尿液中几种常见苯丙胺类药物的GC/MS分析方法

目的:建立能同时对尿液中几种常见苯丙胺类药物进行定性和定量分析的方法。方法:含有苯丙胺类药物的尿液经液液提取(LLE)之后,采用GC/MS技术,以4-苯基丁胺为内标,采用EI,SIM方式,对尿液中的几种苯丙胺类提取物同时进行定性与定量分析。结果:4种苯丙胺类药物在尿药浓度为0·025-3·2μg·ml-1范围内标准曲线的线性关系良好(r=0·9977-0·9998);高、中、低3种浓度各标准药物的回收率较高;日内、日间精密度的RSD(%)基本符合小于10%的要求;最低检测浓度能够达到纳克级,具有较高的灵敏度。结论:本方法可满足尿样中苯丙胺类药物的定性与定量研究,能够用于实际工作中对药物滥用嫌疑者尿样的确证。     

MDMA在急性中毒大鼠体内的分布研究

目的:建立3,4-亚甲基二氧基甲基苯丙胺(MDMA)大鼠急性中毒模型,研究MDMA在大鼠体内的分布情况。方法:按30mg·kg-1给予实验大鼠MDMA盐溶液,灌胃(ig),2h后脱臼处死。运用乙醚萃取衍生化法和气/质联用技术(GC/MS),对大鼠体内各组织和血液中的MDMA进行定性定量分析。结果:急性中毒大鼠体内各组织和血液中MDMA浓度大小依次是:脾>胃>肺>肝>肾>脑>心肌>心血。结论:MDMA广泛分布于大鼠体内各组织及血液中,对这些组织均有潜在的毒害。     

混合滥用药物的气相色谱质谱分析

目的 :建立混合滥用药物快速、灵敏检测方法。方法 :采用气相色谱 质谱法 (GC MS)对 11种毒品、药品进行定性定量分析。结果 :苯丙胺类及吗啡在 5 0× 10 - 4- 2 0× 10 - 2 g·ml- 1 范围内线性关系良好 ,检出限分别为 1 0×10 - 4g·ml- 1 和 2 0× 10 - 4g·ml- 1 ;氯胺酮、哌替啶、地西泮、咖啡因、可卡因、马来酸氯苯吡及乙酰替乙氧苯胺线性范围为 5 0× 10 - 6 - 5 0× 10 - 4g·ml- 1 ,检出限为 1 0× 10 - 6 g·ml- 1 和 2 0× 10 - 6 g·ml- 1 。结论 :本方法可用于混合滥用药物组分的快速、准确定性定量分析。     

气-质联用结合衍生化法分析血浆中甲基苯丙胺和氯胺酮

目的:考察家兔血浆中甲基苯丙胺和氯胺酮同时衍生化后GC/MS检测分析结果。方法:血浆样品中加入内标物丙基解痉素(SKF525A)后碱化,乙醚萃取,三氟醋酸酐(TFA)衍生化,GC/MS全扫描定性、内标法和工作曲线法定量分析。结果:甲基苯丙胺和氯胺酮在血浆中的线性检测范围分别为0.010 0~10.0μg.mL·1和0.010 0~20.0μg.mL·1;方法回收率为95.26%~101.10%;日内及日间相对标准差均小于15%。结论:建立了衍生化后同时测定血浆中甲基苯丙胺及氯胺酮的GC/MS定性定量分析方法,该法简便、灵敏、重复性好,适用于甲基苯丙胺和氯胺酮混合滥用中毒案例的快速鉴定。     

高效液相色谱法梯度洗脱测定三七中三七皂苷R1含量

目的 :以HPLC梯度洗脱测定三七中三七皂苷R1含量。方法 :采用SphericorbNH2 柱 ,流动相为CH3CN CH3OH H2 O ,梯度洗脱浓度 5 5∶30∶15→ 70∶2 0∶10 ,波长 2 10nm ,外标一点法测定。结果 :以峰面积计算 ,三七皂苷R1在 5～ 40 μg·ml-1呈线性相关 ,γ =0 .994,最低检测限为 0 .6 μg·ml-1(S/N =3)。平均回收率 10 2 .6 % ,RSD为 1.43 % .日内误差RSD =1.7% (n =5 ) ,日间误差RSD =3 .0 % (n =4)。结论 :本法专属性强 ,结果准确 ,操作简捷     

HPLC法测定阿莫西林克拉维酸钾分散片的含量

采用HPLC法测定阿莫西林克拉维酸钾分散片的含量。用PhenomenexC18(4 6× 15 0mm 5 μm)色谱柱;甲醇 -0 0 5 7mol·L-1磷酸二氢钠缓冲液(用磷酸或 10N的氢氧化钠调pH值至 4 4± 0 1)(5∶95 )为流动相;检测波长为 2 2 0nm。阿莫西林在 4 0 4 8～ 2 0 2 4 0 μg·ml-1浓度范围内呈良好线性(r =0 9999),最低检出限 0 0 4ng;克拉维酸在 4 0 0 8～ 2 0 0 4 0 μg·ml-1浓度范围内呈良好线性(r =0 9999),最低检出限 0 0 8ng。阿莫西林及克拉维酸钾的回收率分别为 10 0 1%( RSD =0 6 8%)和 99 8% ( RSD =1 2 6 %)     

尼扎替丁的含量及有关物质测定方法的改进

目的　改进美国药典中尼扎替丁有关物质及含量测定方法的条件。方法　采用等度洗脱法进行测定 ,以甲醇 - 0 .0 5mol·L-1乙酸铵缓冲液 (2 0∶80 )为流动相 ,柱温 30℃ ,检测波长 2 5 4nm ,进样浓度 4 5 0 μg·ml-1,进样量 2 0 μl,流速 1.0ml·min-1。有关物质检查和含量测定同时进行。结果　尼扎替丁在 0 .2 8～ 75 0 μg·ml-1范围内线性关系良好 ,最低检出限为 4 .5ng,高、中、低浓度精密度试验RSD分别为 0 .0 2 %、0 .0 2 %、0 .0 3%。结论　方法简便 ,结果准确。     

RP-HPLC法测定人血浆中格列齐特浓度

本文采用反相高效液相色谱法测定人血浆中格列齐特浓度.固定相:ODS-C18;流动相:乙腈-甲醇-水(35:20:45)的混合溶液,并用磷酸调节pH至3.5;流速:1.0 ml·min-1;紫外检测波长:228 nm;方法回收率大于95%,日内、日间相对标准偏差小于8%.血浆的最低检测限为0.05 μg·ml-1;线性范围:0.5～12 μg·ml-1,r＝0.9995.     

尿样中滥用药物的检测分析

目的·· :检测尿样中滥用药物的种类。方法·· :采用胶体金法检测试剂盒和药毒物广筛鉴定检验A系统 (TOXI -LABASYSTEM )对药物滥用嫌疑者尿样进行分析。结果·· :试剂盒检测发现 ,21例中有甲基苯丙胺阳性6例、苯丙胺阳性5例、甲基苯丙胺和苯丙胺均阳性2例、吗啡阳性4例。进一步经TOXI-LAB检测,发现滥用的兴奋剂分别是甲基苯丙胺、亚甲基二氧基苯丙胺 (MDA)或二者混合。结论·· :在检测的尿样中,滥用药物有阿片类药物以及甲基苯丙胺和/或MDA中枢兴奋剂     

一种快速灵敏的血浆吗啡浓度气质联用检测方法

目的 :建立一种快速灵敏的气质联用测定血浆吗啡浓度的方法。方法 :以纳洛芬作内标 ,联合采用固相萃取和PFPA衍生化对血浆吗啡进行气质联用检测。吗啡和纳洛芬的特征质荷比分别为 4 14和 4 4 0 ,保留时间 5 3min和 6 1min。结果 :吗啡标准曲线在 0 0 2 2 - 2 2 μg·ml- 1 浓度范围内具有良好的相关性 (R2 >0 99) ,回收率范围为91% - 98% ,日内精密度 2 4 % - 6 0 % ,日间精密度 2 3% - 7 0 % ,最低检测线 1ng·ml- 1 。结论 :该方法简便可行、准确灵敏 ,可用于药物滥用检测。     

Simultaneous identification of amphetamine and methamphetamine using solid-phase extraction and gas chromatography/nitrogen phosphorous detection or gas chromatography/mass spectrometry

A method for the simultaneous detection and quantitation of amphetamine and methamphetamine in urine is described. Using solid-phase extraction, amphetamine, methamphetamine, and n-propylamphetamine (internal standard) are extracted from urine samples. Drugs in their free form are identified using gas chromatography/nitrogen-phosphorous detection (GC/NPD), whereas their heptafluorobutyric anhydride derivatives are detected by gas chromatography/mass spectrometry (GC/MS) in the selected ion monitoring (SIM) mode. Limits of detection for both amphetamine and methamphetamine are approximately 35 ng/mL. The procedure is simple, rapid, and suitable for a large number of specimens (25 or more).     

Oral fluid with three modes of collection and plasma methamphetamine and amphetamine enantiomer concentrations after controlled intranasal l‐methamphetamine administration

Methamphetamine is included in drug testing programmes due to its high abuse potential. d‐Methamphetamine is a scheduled potent central nervous system stimulant, while l‐methamphetamine is the unscheduled active ingredient in the over‐the‐counter nasal decongestant Vicks® VapoInhaler?. No data are available in oral fluid (OF) and few in plasma after controlled Vicks® VapoInhaler? administration. We quantified methamphetamine and amphetamine enantiomers in OF collected with two different devices and plasma via a fully validated liquid chromatography‐tandem mass spectrometry (LC‐MS/MS) method. Additionally, OF were analyzed with an on‐site screening device. Sixteen participants received 7 Vicks® VapoInhaler? doses according to manufacturer's recommendations. Specimens were collected before and up to 32 h after the first dose. No d‐methamphetamine or d‐amphetamine was detected in any sample. All participants had measurable OF l‐methamphetamine with median maximum concentrations 14.8 and 16.1 μg/L in Quantisal? and Oral‐Eze® devices, respectively, after a median of 5 doses. One participant had measurable OF l‐amphetamine with maximum concentrations 3.7 and 5.5 μg/L after 6 doses with the Quantisal? and Oral‐Eze® devices, respectively. There were no positive DrugTest® 5000 results. In the cutoff range 20–50 μg/L methamphetamine with amphetamine ≥limit of detection, 3.1–10.1% of specimens were positive; first positive results were observed after 1–4 doses. Two participants had detectable plasma l‐methamphetamine, with maximum observed concentrations 6.3 and 10.0 μg/L after 2 and 5 doses, respectively. Positive OF and plasma methamphetamine results are possible after Vicks® VapoInhaler? administration. Chiral confirmatory analyses are necessary to rule out VapoInhaler? intake. Implementing a selective d‐methamphetamine screening assay can help eliminate false‐positive OF results. Published 2015. This article is a U.S. Government work and is in the public domain in the USA.     

Quantitation of methamphetamine and amphetamine in urine by capillary GC/MS. Part I. Advantages of trichloroacetyl derivatization

A urine assay for methamphetamine and amphetamine that is compatible with our existing high-volume GC/MS assays for other drugs of abuse has been developed. Trichloroacetic anhydride is used for derivatization and its derivative is substantially less volatile than other commonly used derivatives. The internal standard is the primary amine 2-methylphenethylamine. The procedure utilizes an initial liquid-liquid extraction, a liquid-liquid back extraction for specimen cleanup, and derivatization for removal of excess trichloroacetic anhydride and acid by-product. A GC temperature of about 180 degrees C results in retention times of approximately 2.8, 3.2, and 4.3 min for amphetamine, the internal standard, and methamphetamine, respectively. Five ions are monitored: 91+, 118+, 188+ for amphetamine; 105+, 118+ for 2-methylphenethylamine; and 91+, 118+, 202+ for methamphetamine. Full scan GC/MS data from a variety of other derivatives are examined and used to illustrate the advantages of derivatizing molecules with strongly electronegative atoms near the reaction site. This situation forces fragmentation patterns in which positive charges are located on larger and structurally acceptable identifying mass fragments of the original methamphetamine or amphetamine molecule.     

多种尿检试纸联用结合GC/MS确认方法对所谓“摇头水”的检测

目的··∶研究出一种既能区别“摇头水”、摇头丸和海洛因 ,又能在现场快速检测的方法。方法··∶用吗啡、苯丙胺、甲基苯丙胺胶体金抗体试纸分别对“摇头水”、摇头丸和海洛因进行初步分类检验 ,并将尿液通过固相萃取柱进行提取 ,所得提取液再用GC/MS进一步确证。结果··∶3种试纸联用 ,经不同结果的组合 ,可以在现场查验中快速排除阴性对象 ,筛选出嫌疑对象 ;通过GC/MS的确证实验 ,可以进一步区别海洛因吸食者和“摇头水”滥用者的尿液。结论··∶多种尿检试纸联用结合GC/MS确认 ,是一个快速、准确、可行的现场检测尿液中毒品的方法。     

Choice of an ELISA assay for screening postmortem blood for amphetamine and/or methamphetamine

The object of this study was to evaluate the suitability of the Neogen Corp. microtiter plate enzyme-linked immunoassays (ELISA) for the screening of postmortem blood for amphetamine and methamphetamine and to choose the more appropriate assay for screening. Forty-seven postmortem whole blood specimens were obtained from drug-involved deaths, which had been screened and confirmed positive for methamphetamine and/or amphetamine. Eighty-five negative specimens were obtained from non-amphetamines-involved deaths, 17 of which involved decomposition. Specimens were tested using the Neogen Amphetamine Ultra and Neogen Methamphetamine/MDMA microtiter plate ELISA assays. No matrix effects were found for whole blood in these assays, and a dilution of 1:5 was chosen to facilitate pipetting and to bring the IC50 of the microtiter plate ELISA assay within the range of amphetamines concentrations encountered in medical examiner specimens. True positives, true negatives, false positives, and false negatives were determined relative to gas chromatography-mass spectrometry (GC-MS) and graphed for the ELISA. From these graphs and the receiver operating curves (ROC), the optimal cut-off for the Neogen Methamphetamine/MDMA ELISA was 50 ng/mL methamphetamine equivalents and the optimum cut-off for the Neogen Amphetamine Ultra ELISA was 100 ng/mL amphetamine equivalents. The Neogen Methamphetamine ELISA had a sensitivity of 93.6% +/- 3.5% and a specificity of 77.6% +/- 4.5% versus GC-MS at the cut-off of 50-ng/mL methamphetamine equivalents. The Neogen Amphetamine Ultra ELISA had a sensitivity of 95.7% +/- 3.0% and a specificity of 72.9% +/- 5.2% versus GC-MS at the 100-ng/mL amphetamine equivalents cut-off. The areas under the ROCs were equivalent for the two ELISA assays.     

液相色谱-串联质谱法测定人血浆中的米氮平及在药动学中的应用

目的:研究液相色谱-串联质谱法测定人血浆中的米氮平,并应用于生物等效性研究。方法:50μL 血浆样品经乙腈沉淀蛋白处理后,以乙腈-水-甲酸(80:20:0．2)为流动相,Zorbax SB-C_8柱分离,采用电喷零离子源,选择反应监测方式进行正离子检测。用于定量分析的离子反应分别为m／z 266→195(米氮平)和 m／z 256→167(内标,苯海拉明)。药动学参数采用非室模型计算。结果:米氮平测定方法的线性范围为0．18- 144．0 μg·L~(-1),定量下限为0．18 μg·L~(-1)。日内、日间精密度(RSD)均小于6．2％,准确度(RE)在±2．0％以内。每个样品测试时间仅为3．5 min。口服米氮平片30 mg后测得参比制剂和受试制剂的t_(max)分别为(1．4±s 0．7)h 和(1．4±0．7)h,c_(max)分别为(65±35)μg·L_(-1)和(69±35)μg·L_(-1),t_(1/2)分别为(24±6)h和(24±6)h,用梯形法计算,AUC_(0-96)分别为(814±419)μg·h·L_(-1)和(842±387)μg·h·L_(-1)。以AUC_(0-96)计算,受试制剂相对生物利用度为(102±18)％。结论:该法选择性强、灵敏度高、操作简便,适用于米氮平的制剂的生物等效性评价及临床药动学研究。     

川芎哚药代动力学参数的稳定同位素法测定

目的　测定川芎哚 (川芎III号碱 ,perlolyrine)的药动学参数。方法　以氘标川芎哚为内标准及GC MS的SIM(选择性离子监测 )为检测手段 ,定量测定大鼠体内川芎哚的含量及其药代动力学参数。结果　川芎哚在大鼠体内呈二室模型分布 ,其药代动力学参数为 :T1/ 2α=0 34h ,T1/ 2 β=4 5 9h ,T1/ 2 (Ka) =0 12h ,Tmax=0 36h ,Cmax=18 86μg·L-1,K12 =0 87h-1,K2 1=0 40h-1,K10 =0 31h-1,VB=10 7 86L·kg-1,AUC =99 6 8μg·h·L-1。结论　本法灵敏度高、特异性强和准确性好 ,为临床应用提供了科学依据。