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目的建立了新型微流体液相色谱(micro-LC)串联四级杆质谱检测头发中5种苯二氮卓类药物(三唑仑,α-羟基咪达唑仑,咪达唑仑,α-羟基阿普唑仑,普拉西泮)。方法采用液-液萃取法(LLE)提取毛发样品,微流体液相色谱串联四级杆质谱检测。结果在回归系数大于0.99的情况下,目标分析物的良好线性。精密度和萃取效率分别在2.7%~17.1%和66.5%~120.5%之间。每个分析物的检出限和定量限分别为0.001~0.08 pg·mg^-1和0.0125~0.25pg·mg^-1。结论本方法与传统的液相色谱串联质谱法(LC/MS-MS)相比灵敏度出高2-10倍。本研究展示了新型微流体分离系统串联质谱方法的实用性,并为法医毒理学领域关于头发样本中痕量药物检测提供了一种新的检测手段。 相似文献
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目的建立生物检材包括血、肝组织、胃组织中阿维菌素(Avermectins)的HPLC—MS/MS分析方法。方法采用Oasis HLB固相萃取柱进行提取,以XTerra^TM RP18柱(2.1mm×100mm,3.5μm)色谱柱分离,以甲醇-0.1%冰醋酸水溶液(75:25)为流动相,流速为0.2mL/min。结果线性范围10ng/mL~3μg/mL,最小检出限为0.1ng/mL。结论本方法准确、快速,可用于生物检材血中阿维菌素的定性定量分析,肝及胃组织中阿维菌素的定性分析。 相似文献
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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。 相似文献
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目的建立人体全血中五氟利多浓度的液相色谱-质谱联用法(LC-MS/MS)分析方法。方法全血中五氟利多和利培酮(内标)经正己烷液-液提取后,采用Capcell Pak C18色谱柱(250mm×2.0mm5,μm)进行分离,流动相为乙腈:20mmol/L乙酸胺和0.1%甲酸溶液(75∶25,V/V),流速为0.2mL/min,然后以MS/MS电喷雾正电离的多反应监测扫描方式(MRM)测定。用于定量分析的离子为m/z 524→109(五氟利多)和m/z 411→191(内标)。结果五氟利多的最低检测限为0.2ng/mL,在0.4~400ng/mL浓度范围内线性良好(r=0.9994),低、中、高浓度(1ng/mL、10ng/mL、100ng/mL)准确度分别为97%,108%和95%,日内和日间RSD均小于15%。结论该方法简便、快速、灵敏,适用于全血中五氟利多浓度的测定。 相似文献
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6-Monoacetylmorphine (6-MAM) is a good indicator for the intake of heroin and can be detected in blood, urine and hair of heroin users. A new radioimmunoassay (RIA) designed specifically for 6-monoacetylmorphine (6-MAM) was tested for its usefulness for the quantitation of the drug in urine, serum and hair. Its cross-reactivity with heroin and its metabolites, and related compounds was also determined. Eighty-nine hair, six serum and 25 urine samples where 6-MAM had been previously identified by GC/MS were analysed for 6-MAM with the new RIA kit. A good correlation existed between the GC/MS and RIA results for the hair samples. However, the amount of 6-MAM found in serum and urine differed considerably between the two methods. This difference could be explained by the cross-reactivity of the antibody with morphine and morphine-6-glucuronide, which are present in much larger amounts in serum and urine, than in hair. To evaluate a new rationalisation procedure, some hair samples were split into two portions after incubation. One part was analyzed for 6-MAM by RIA, and the other portion by GC/MS. 相似文献
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生物检材中乌头碱的LC-MS/MS快速分析 总被引:1,自引:1,他引:0
目的应用高效液相色谱-质谱法对生物检材中乌头生物碱等有毒成分进行快速分析。方法取全血样品经乙腈-甲醇(5:1 v/v)提取,使用Agilent Zorbax SB C18(2.1 mm×50 mm,1.8μm)色谱柱,以0.1%甲酸溶液-乙腈(60:40 v/v)为流动相等度洗脱。在多反应监测模式下测定全血样品中乌头生物碱等有毒成分。结果乌头碱、次乌头碱和中乌头碱的保留时间为0.73 min、0.77 min和0.63 min;用于定量分析的离子对分别为m/z 646.4→586.4(乌头碱)、616.1→556.5(次乌头碱)和632.4→572.1(中乌头碱)。乌头碱在0.1~250 ng/m L内线性关系良好,相关系数(r)≥0.9987,最低检出限0.1ng/m L,精密度考查其变异系数(CV)5.42%(n=6),血液中乌头碱提取回收率不小于90%。结论本文建立的高效液相色谱-质谱法快速、简便、灵敏,适用于天然药毒物检验。 相似文献
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Concheiro M Simões SM Quintela O de Castro A Dias MJ Cruz A López-Rivadulla M 《Forensic science international》2007,171(1):44-51
A fast method was designed for the simultaneous determination of amphetamine (A), methamphetamine (MA), PMA, MDA, MDMA, MDEA and MBDB in urine. The drugs were analysed by LC (ESI)-MS/MS, after a simple liquid-liquid extraction in the presence of the deuterated analogues. Reverse phase separation on an Atlantis dC18 Intelligent Speed column was achieved in less than 4 min under gradient conditions, and the total run time was 8 min. The method was fully validated, including linearity (1-1000 ng/mL for A, MDMA, MDEA and MBDB; 2-1000 ng/mL for MDA and PMA; 1-200 ng/mL for MA; r2>0.99 for all compounds), recovery (>80%), within-day and between-day precision and accuracy (CV and MRE<12.7% for intermediate level and ULOQ, and <17.2% for LLOQ), limit of detection (0.2 ng/mL for MDMA, MDEA and MBDB; 0.5 ng/mL for A, MA and PMA; 1 ng/mL for MDA) and quantitation (1 ng/mL for A, MA, MDMA, MDEA and MBDB; 2 ng/mL for MDA and PMA) and relative ion intensities. No matrix effect was observed. The procedure proved to be sensitive, specific and rapid, and was applied to real forensic cases. 相似文献
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目的建立一种检验生物检材中无机氰化物的GCMS/MS方法。方法首先将生物检材中的无机氰化物在酸性条件下蒸馏出,用碱性溶液吸收后,氰离子在相转移催化剂作用下被五氟苄基溴(PFB-Br)衍生化,最后用GC-MS/MS法分析衍生化产物。结果衍生化产物PFB-CN的MS/MS质谱图特征性强,定性准确;在20-1500ng/g浓度范围内呈良好的线性关系(r=0.998),最低检测限为5ng/g,回收率为82.3%-98.6%。结论本方法简单实用,灵敏度高,准确可靠,适用于生物检材中无机氰化物的检验。 相似文献
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目的 采用气相色谱/质谱法检测人体血液和肾、肝组织中的丙泊酚.方法 心血和肾、肝组织中的丙泊酚经环己烷提取,采用气相色谱/质谱法,丙泊酚选择m/z 163、178,内标百里香酚选择m/z 150、135进行测定;并考察方法专属性、线性范围、定量线与检出限、回收率与精密度.结果 丙泊酚的保留时间为8.17min,与内标百里香酚分离良好;其在心血和肾、肝组织中的检测浓度线性关系良好,r值均大于0.992,最低检测质量浓度分别为0.05 μg/mL、0.10μg/g及0.05 μg/g,方法回收率90% ~ 110%,日内、日间RSD均小于7%.结论 本文方法简便、灵敏、快速,其准确度、精密度和回收率均可满足生物检材中丙泊酚浓度的测定,可在相关研究及实践中选用. 相似文献
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目的研究生物组织中两种混合农药(敌敌畏、克百威)的痕量确认方法;方法采用时间编程方法和GC-CI-MS/MS技术,选择在共振方式下,用CI化学源在4min~6.5min以敌敌畏的分子离子(M 1)221为母离子进行MS/MS分析;结果其碰撞诱导电压为0.5v,产生的二级质谱子离子为141,145;在6.5min~13min以克百威的分子离子(M 1)222为母离子进行MS/MS分析,其碰撞诱导电压为0.4v,产生的二级质谱子离子为165,123;结论排除背景干扰、定性快而准确。 相似文献
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目的建立血液、尿液以及肝中河豚毒素(tetrodotoxin,TTX)的液相色谱-串联质谱分析方法,并进行方法学验证。方法血液、尿液和肝用1%乙酸甲醇溶液去蛋白后,上清液用固相萃取法净化,LC-MS/MS检测。结果血液、尿液和肝中TTX检出限分别为2ng/mL、2ng/mL和4ng/g。血液和尿液在4~100ng/mL、肝在5~100ng/g的范围内线性关系良好,相关系数r≥0.9973;日内精密度和日间精密度均在12.80%以内;回收率大于47.2%。结论所建方法高效、灵敏、准确,可以为河豚毒素中毒的法医学鉴定、临床诊治以及食品安全的监控提供技术保障。 相似文献
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Marjorie Chze Marc Deveaux Claire Martin Michel Lhermitte Gilbert Ppin 《Forensic Science International Supplement Series》2007,170(2-3):100
A rapid and sensitive method using LC-MS/MS triple stage quadrupole for the determination of traces of amphetamine (AP), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA, “ecstasy”), 3,4-methylenedioxyethamphetamine (MDEA), and N-methyl-1-(3,4-methylenedioxyphenyl)-2-butanamine (MBDB) in hair, blood and urine has been developed and validated. Chromatography was carried out on an Uptisphere ODB C18 5 μm, 2.1 mm × 150 mm column (Interchim, France) with a gradient of acetonitrile and formate 2 mM pH 3.0 buffer. Urine and blood were extracted with Toxitube A® (Varian, France). Segmented scalp hair was treated by incubation 15 min at 80 °C in NaOH 1 M before liquid–liquid extraction with hexane/ethyl acetate (2/1, v/v). The limits of quantification (LOQ) in blood and urine were at 0.1 ng/mL for all analytes. In hair, LOQ was <5 pg/mg for MA, MDMA, MDEA and MBDB, at 14.7 pg/mg for AP and 15.7 pg/mg for MDA. Calibration curves were linear in the range 0.1–50 ng/mL in blood and urine; in the range 5–500 pg/mg for MA, MDMA, MDEA and MBDB, and 20–500 pg/mg for AP and MDA. Inter-day precisions were <13% for all analytes in all matrices. Accuracy was <20% in blood and urine at 1 and 50 ng/mL and <10% in hair at 20 and 250 pg/mg. This method was applied to the determination of MDMA in a forensic case of single administration of ecstasy to a 16-year-old female without her knowledge during a party. She suffered from hyperactivity, sweating and agitation. A first sample of urine was collected a few hours after (T + 12 h) and tested positive to amphetamines by immunoassay by a clinical laboratory. Blood and urine were sampled for forensic purposes at day 8 (D + 8) and scalp hair at day 60 (D + 60). No MDMA was detected in blood, but urine and hair were tested positive, respectively at 0.42 ng/mL and at 22 pg/mg in hair only in the segment corresponding to the period of the offence, while no MDA was detectable. This method allows the detection of MDMA up to 8 days in urine after single intake. 相似文献
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目的采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC/MS/MS)检测人唾液中地西泮及其代谢物。方法采用固相萃取法(SPE)处理唾液,HPLC/MS/MS法检测,MRM记录方式,保留时间和定性离子对定性,内标法和标准曲线法定量。结果地西泮及其代谢物去甲地西泮、去甲羟基西泮、去甲羟基地西泮葡萄糖醛酸苷(OG)、羟基地西泮葡萄糖醛酸苷(TG)的检测限在0.01ng/m L~0.5ng/m L之间,线性范围0.1ng/m L或0.5ng/m L~100ng/m L,回收率为84.9%~106%。口服5mg地西泮后15d内唾液中可检出地西泮及去甲西泮,但检出时间有个体差异,但去甲羟基西泮、TG和OG则不能检出。结论 SPE-HPLC/MS/MS检测法可应用于人唾液中地西泮及其代谢物的检测。人口服常量地西泮后唾液中可检出地西泮和去甲西泮,且检测窗口期较宽,但存在个体差异。 相似文献
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目的建立一种简单、快速测定生物检材(血液、尿液、胃内容物)乌头碱的超高效液相色谱-质谱联用法。方法样品采用乙腈沉淀处理。色谱柱为UPLC C18(2.1mm×50mm,1.7μm),流动相为乙腈-0.1%甲酸,梯度洗脱,流速为0.4m L/min,柱温40℃。采用ESI离子源,MRM模式检测。结果乌头碱在血液0.5~500ng/m L,尿液1~1000ng/m L浓度范围内线性良好(r>0.995)。乌头碱方法回收率在91.3%~110.2%之间;提取回收率在72.8%~83.5%之间;日内、日间RSD均小于14%。结论本方法简单、快速检测生物检材中乌头碱。 相似文献
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LC-MS/MS法测定人血浆中盐酸洛哌丁胺 总被引:1,自引:0,他引:1
目的建立人血浆中盐酸洛哌丁胺的液相色谱-质谱联用测定法(LC-MS/MS)。方法血浆样品中盐酸洛哌丁胺与盐酸小檗碱(内标)经甲醇液.液提取后,采用ZORBAXSB—C18色谱柱(2.1mm×150mm×5μm),柱温35℃,流动相为乙腈:0.1%甲酸(60:40,V/V),流速为0.4mL/min,进样量10μL。电喷雾离子源(ESI),正离子检测,以多反应监测(MRM)方式进行定量分析,用于监测的离子为m/z477→266(盐酸洛哌丁胺)和m/z366→292(内标)。结果盐酸洛哌丁胺的检测下限为0.2ng/mL(S/N=3),在浓度0.5~500ng/mL范围内线性良好(r=0.9982),低、中、高浓度(1ng/mL、20ng/mL、400ng/mL)的平均回收率分别为84.6%,88.5%和90.2%,日内与日问RSD分别小于6%与7%。结论LC—MS/MS法可用于盐酸洛哌丁胺的定性定量分析。 相似文献
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A method for the sensitive and selective determination of ethyl glucuronide (EtG) in hair has been developed using solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Washed and cut hair segments were extracted by ultrasonication (3h, 50 degrees C) and the extracts were cleaned-up with aminopropyl SPE columns. LC-MS/MS analysis was performed using a polar-endcapped phenyl-hexyl-RP-phase with negative mode electrospray ionisation (ESI) using a triple quadrupole mass spectrometer (Sciex API 365) with a turboionspray source and post-column addition of acetonitrile for enhanced sensitivity. The MS/MS transitions monitored were m/z 221 -->75 for EtG and 226 -->75 for D(5)-EtG as an internal standard. The method was selective and sensitive, with a detection limit of 51 pg/mg hair at a signal-to-noise ratio of 3:1. The mean recovery was 96%, with an intra- and inter-day precision of less than 11.7% at a concentration of 200 pg/mg. The linearity was assessed in the range of 25-2000 pg/mg hair, with a correlation coefficient of 0.997. The method was successfully applied to 97 human hair samples which were taken at autopsies from persons with known alcoholism or were obtained from alcoholics who were hospitalized for ethanol withdrawal, from social drinkers and from children having not consumed any alcohol. Although, approximately two-third of the alcoholics showed EtG concentrations in hair of higher than 51 pg/mg (up to >4000 pg/mg), in one-third the EtG concentration was below the detection limit. However, only in one of five hair samples of "social drinkers", the EtG concentration was above the detection limit (51 pg/mg). No EtG has been detected in the hair of children. These investigations demonstrate that heavy alcohol consumption may be but not necessarily has to be detectable by EtG analysis in hair. 相似文献
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目的建立定量分析人全血中马钱子碱和士的宁的高效液相色谱质谱联用法。方法应用Oasis^TM MCX小柱进行固相萃取法提取,XTerra^TM RP18色谱柱分离。结果在该条件下,人血中马钱子碱和士的宁的线性范围为0.01—5.0μg/ml,最小检出限为0.2ng/ml;马钱子碱和士的宁在0.01—5.0μg/ml浓度范围内的回收率均在80%以上。结论高效液相色谱质谱联用法可定量测定血中马钱子碱和士的宁。 相似文献
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固相微萃取(SPME)GC/MS、GC/MS/MS法检测环境水中的有机磷杀虫剂 总被引:11,自引:0,他引:11
目的 通过对固相微萃取 (SPME)条件的优化、筛选实验 ,建立环境水中有机磷杀虫剂的快速检验方法。方法 收集 17种有机磷杀虫剂 ,使用SPME并结合GC/MS、GC/MS/MS检验方法。结果 该方法简便、灵敏、迅速、可靠 ,样品利用率高 ,最低检测浓度为 0 .0 1~ 10 0 pg/ml,在痕量范围 0 .1~ 10ng/ml内线性回归好(相关系数r达 0 .99以上 )。结论 实际应用效果理想 ,有望成为公安、环保、检验检疫的农残及毒物分析中的一种快速有效的分析方法。 相似文献