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液相色谱-质谱联用技术在毒物分析中的应用 总被引:1,自引:0,他引:1
本文简要综述了液-质(LC-MS)联用的基本结构以及该技术近年来在滥用药物、治疗药物和杀虫剂中的应用,为进一步扩大液-质联用技术在毒物分析领域中的应用提供参考. 相似文献
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目的建立尿液中15种常见安眠镇静药物及代谢物的液相色谱-串联质谱分析方法。方法尿液经酶水解、固相萃取后,用C18液相柱分离,以含甲酸铵和甲酸的水、乙腈为流动相梯度洗脱,质谱采用电喷雾电离(ESI)-正负离子模式同时扫描,采用二级质谱多反应监测(MRM)模式检测目标化合物。结果以化合物的保留时间、两对母离子/子离子对定性,尿中常见安眠镇静药物的检测限为0.01~0.5ng/mL(ESI+)和10ng/mL(ESI-);相关系数r在0.994以上;日内及日间精密度均在18%以下;绝对回收率在64.80%~116.20%之间。结论方法快速、灵敏、简便、可靠,能同时分析尿液中的15种安眠镇静药物及其代谢物。 相似文献
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甲苯噻嗪的检验1例 总被引:1,自引:0,他引:1
“甲苯噻嗪”是一种兽用止痛药,有麻醉作用,将其用于对人体实施麻醉犯罪,少见报道。甲苯噻嗪化学名为5,6-二氢-2-(2,6-二甲苯胺基)-4H-1,3-噻嗪,为结晶,熔点135~138℃。盐酸甲苯噻嗪为白色粉末,熔点164℃~167℃。易溶于水、乙醇和甲醇,微溶于乙醚和氯仿犤1犦。毒性LD50(口服)小鼠240mg/kg,大鼠130mg/kg。大白鼠口服实验证明,其迅速并几乎被完全吸收。药物迅速被代谢生成近20种代谢产物,代谢最终产物为无机硫酸盐和二氧化碳,仅有剂量的8%以原形从尿中排出。剂量的70%从尿中排泄,30%从粪便中排泄。10~15小时后排泄完全。1提取方法原药或… 相似文献
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UPLC-MS/MS检测人血中18种有机磷及氨基甲酸酯类农药 总被引:2,自引:2,他引:0
目的建立人血中18种有机磷及氨基甲酸酯类农药超高压液相色谱-串联质谱(UPLC-MS/MS)的检测方法。方法血液中加入乙腈沉淀蛋白,采用Waters BEH C18(1.7μm 2.1×50mm)柱子,流动相为5mmol/L乙酸铵水-甲醇,流速:0.3m L/min;进样量:2μL,电喷雾离子源(ESI),正离子检测,采用多反应监测方式进行定量分析。结果药物最小检测限(LOD)在0.1~40ng/m L之间,定量限(LOQ)在0.5~50ng/m L之间,各药物浓度在定量限到500ng/m L范围内线性良好,回收率均在64.3%~111.9%之间,相对标准偏差为3.9%~10.3%。结论该方法专属性强、灵敏、准确,可以适用于法庭与临床毒物分析。 相似文献
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A simple and rapid method for the isolation of seven synthetic pyrethroid insecticides (methothrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, fenvalerate, deltamethrin) with a solid phase extraction (SPE), utilizing Sep-Pak C18 cartridges, from human urine and plasma is presented. The detection of the insecticides was performed using a wide bore capillary gas chromatograph (GC) with flame ionization detection (FID). The insecticide-containing samples mixed with 70% methanol were directly applied to the cartridges and eluted with 2 ml chloroform. The recoveries using the cartridges were between 90-102% for urine and 81-93% for plasma. Mixing samples with 70% methanol prior to extraction, seems very useful for the screening of synthetic pyrethroid insecticides. 相似文献
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A rapid and precise method for the isolation and identification of dihydrocodeine from urine is reported. The narcotic is isolated from urine using Sep-Pak C18 cartridges for cleanup, requiring less than 30 min for preparation. Identification is performed by gas chromatography/mass spectrometry. 相似文献
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A rapid method for isolation of various benzodiazepines from human samples with Sep-Pak C18 cartridges before wide-bore capillary gas chromatography is described. The drugs dissolved in alkaline samples were directly applied to the cartridges and eluted with hexane/isopropanol (9:1). The recoveries were excellent for all drugs in urine samples, but were somewhat lower for some drugs in plasma samples. The latter problem could be easily circumvented by using a deproteinization process before their application to the cartridge. We can recommend the Sep-Pak C18 cartridges for isolation of benzodiazepines because of their simplicity and rapidity. 相似文献
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A simple and rapid method, for the isolation of eight triazine herbicides from human serum and urine, using Sep-Pak C18 cartridges is presented. After mixing with distilled water, serum and urine samples containing the herbicides, were loaded on Sep-Pak C18 cartridges and eluted with either chloroform only or chloroform/methanol (9:1). The herbicides were detected by capillary gas chromatography with both flame ionization detection (FID) and nitrogen-phosphorus detection (NPD). Separation of eight triazine herbicides from each other and from impurities was generally satisfactory with the use of a non-polar DB-1 capillary column. Recovery of most compounds was excellent for both chloroform and chloroform/methanol (9:1) as elution solvents. Backgrounds were cleaner and evaporation time was shorter for the chloroform only than for the chloroform/methanol (9:1). The NPD gave sensitivity more than 10-20 times higher than that of FID. 相似文献
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A simple and rapid method for isolation of five butyrophenones with Sep-Pak C18 cartridges from human samples, and their wide-bore capillary gas chromatography (GC), are presented. The GC was made by both flame ionization and electron capture detections. The drugs contained in alkaline samples were directly applied to the cartridges and eluted with chloroform/isopropanol (9:1). The recoveries with use of the cartridges were excellent for most drugs in both urine and plasma samples. We can recommend the Sep-Pak C18 cartridges for isolation of butyrophenones because of simplicity and rapidity, and also wide-bore capillary GC because of high sensitivity and low decomposition of drugs during passage through the column. 相似文献
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Rapid isolation with Sep-Pak C18 cartridges and wide-bore capillary gas chromatography of organophosphate pesticides 总被引:1,自引:0,他引:1
A simple and rapid method for isolation of eleven organophosphate pesticides with Sep-Pak C18 cartridges from human urine and plasma, is presented. The detection of the pesticides was made by wide-bore capillary gas chromatography (GC) with flame ionization detection. The pesticide-containing samples, after mixing with water, were directly applied to the cartridges and eluted with chloroform/isopropanol (9:1). The recoveries with use of the cartridges were excellent for most pesticides. Separation of each pesticide peak from each other and from impurities on the gas chromatograms was also satisfactory with use of non-polar and slightly polar capillary columns. The isolation method with use of the cartridges, together with the wide-bore capillary GC, seems very useful in forensic and environmental chemistry and clinical toxicology. 相似文献
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本文介绍了一种应用Sep—Pak C_(18)固相萃取柱从各类生物检材中快速提取净化9种氨基甲酸酯类农药的方法,并用大口径毛细管气相色谱进行分析。9种药物包括:速灭威、叶蝉散、灭多虫、灭除威、灭杀威、残杀威、巴沙、呋喃丹、西维因。萃取前,水基质检材用蒸馏水稀释;脏器检材加0.4N高氯酸溶液。用3ml氯仿/异丙醇(9:1)洗脱药物。水基质检材的回收率(尿、血浆、全血)在80—100%之间;脏器检材的回收率(肝、肾、脑)在66—100%之间。Sep—Pak C_(18)小柱用于尿和血浆样品时可反复使用。 相似文献
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《Forensic science international》1995,72(3):199-207
A simple and rapid method for the extraction of four diazine herbicides (terbacil, bromacil, norflurazon and PAC) from human whole blood, plasma and urine with use of Bond Elut C18 cartridges is presented. Whole blood, plasma and urine samples containing the herbicides, after mixing with distilled water, were loaded on Bond Elut C18 cartridges and the herbicides were eluted with chloroform/methanol (9:1). They were detected by capillary gas chromatography with flame ionization detection (FID) with splitless injection. Separation of the four diazine herbicides from each other and from impurities was generally satisfactory with the use of an intermediately polar DB-17 capillary column. The recovery of all compounds, which had been added to whole blood, plasma and urine, was > 89%. The calibration curve for the herbicides, which has been added to whole blood, plasma and urine, showed linearity in the range 1.6–100 ng on column. Their detection limits were 1.2–1.4 ng on column for whole blood and plasma, and 1.1–1.2 ng on column for urine. 相似文献
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A method for the quantitative determination of strychnine in biological fluids by gas chromatography--mass spectrometry is proposed. The preparation of samples for the analysis included extraction of strychnine from blood and urine with the use of AccuBond(II) EVIDEX cartridges for solid-phase extraction and SPEC MP3 disks respectively. The efficiency of extraction was estimated at 0.05 mg/l for blood and 0.02 mg/l for urine. The detection limit was 0.10 mg/l in blood and 0.05 mg/l in urine. 相似文献
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固相萃取/LC-MS/MS测定尿液中吗啡类药物 总被引:2,自引:1,他引:1
目的 建立尿液中吗啡类药物的固相萃取/LC—MS/MS方法。方法采用OASIS MCX3cc(60mg)固相萃取柱进行提取,应用LC—MS/MS方法进行检测,运用保留时间和MRM方式对尿液中吗啡类药物及其代谢物进行定性定量分析。结果磷酸盐缓冲液pH4.0时,海洛因、6-MAM、可待因、吗啡、M3G的固相萃取回收率分别达64.33%-70.21%,96.95%~117.57%,83.60%~123.63%,68.82%~91.03%,94.64%~107.33%;最低检测限(LOD)分别为5、10、5、5、2pg,线性范围0.005~10μg/mL;相关系数分别为0.9998、0.9958、0.9992、0.9994、0.9997。结论本文所建方法,适用于尿液中吗啡类药物的分析。 相似文献