共查询到19条相似文献,搜索用时 171 毫秒
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氟乙酸类鼠药包括氟乙酰胺、氟乙酸和氟乙酸钠等。氟乙酰胺和氟乙酸钠都是效力很强的杀鼠剂。氟乙酰胺纯品为白色、无臭、无味的针状结晶,熔点107℃~108℃,受热可升华,170℃分解;溶于水、甲醇、乙醇等溶剂,在二氯甲烷、氯仿、乙醚中的溶解度较小,难溶于石油醚;干燥条件下较稳定,水溶液中能水解成氟乙酸;酸和碱可使水解加速,分别生成氟乙酸和氟乙酸盐。氟乙酸是比醋酸强的有机酸,熔点33℃,沸点165℃,能溶于水和醇。氟乙酸钠又名1080、氟醋酸钠,其纯品为白色结晶,加热至200℃时分解;有吸湿性,极易溶于水,微溶于丙酮、乙醇和油类犤1犦。氟乙酸… 相似文献
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本文建立了离子色谱-抑制电导检测测定含有高浓度硝酸根的爆炸尘土中残留氯酸根的方法。使用高容量阴离子分析柱IonPac AS19,以KOH为流动相,梯度淋洗,氯酸根在8min左右出峰,15min之内完成常规离子的分析,方法的检测限为2.67ng/ml(S/N=3)。方法的线性范围为0.01~1000μg/ml,线性相关系数为0.9998。模拟样品中1μg/mlClO3^-的峰面积相对标准偏差为0.98%,峰高的相对标准偏差为0.66%。将此法应用于两起爆炸案的爆炸尘土样品测定,加标回收率在99%以上。对主要干扰物离子硝酸根的研究发现,即使3000μg/ml的硝酸根对低浓度氯酸根(几个ppm级)的测定也不存在干扰,确保了测定结果的准确性。 相似文献
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人血、尿中富马酸喹硫平的气相色谱分析 总被引:1,自引:0,他引:1
目的建立人血、尿中富马酸喹硫平的气相色谱分析方法。方法用乙醚提取血、尿中的富马酸喹硫平,直接对其进行定性、定量分析。以正常人血、尿为空白样本,分别添加标准富马酸喹硫平,确定检材的前处理方法、色谱分析条件、工作曲线、线性范围、方法的精密度、回收率等,并对1例大剂量服用富马酸喹硫平中毒死者的体液浓度进行测定。结果该方法分析血、尿中富马酸喹硫平的线性范围分别为8.0~800.0μg/ml和20.0—800.0μg/ml;最低检测限分别为0.04μg/ml和0.10μg/ml(S/N≥3),日内、日间精密度均小于4%,回收率在97.08%-101.42%之间。结论该分析方法操作便捷、实用、准确度高,适用于富马酸喹硫平的临床血药浓度快速监测和法医毒物鉴定。 相似文献
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氟乙酸五氟苄基酯的气相色谱分析 总被引:2,自引:0,他引:2
目的 对氟乙酸根阴离子的衍生物-氟乙酸五氟苄基酯(PFB-MFA)进行了气相色谱分析,以满足氟乙酰胺类鼠药化验工作的需要。方法 使用GC/ECD、GC/MS Scan、GC/MS SIM对该化合物的标准溶液进行了分析,得到了各种分析方法的校正曲线及检测限。结果 三种方法测定PFB-MFA的线性范围分别为GC/ECD 0.01~0.1ng/μl、GC/MS SCAN 1~100ng/μl、GC/MS SIM 5×10~(-3)~1ng/μl。三种方法对氟乙酸根阴离子的检测限分别为:GC/ECD1.31×10~(-4)ng/μl、GC/MS SCAN 0.13ng/μl、GC/MS SIM 1.76×10~(-4)ng/μl。结论 氟乙酸根阴离子的衍生物氟乙酸五氟苄基酯在GC/ECD及GC/MS上具有一定的线性范围,有非常高的灵敏度,可用于法庭科学的定性定量分析。 相似文献
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体液中氟乙酰胺SPE-GC/MS检测 总被引:1,自引:1,他引:0
目的 利用GC/MS与固相萃取 (SPE)技术相结合 ,开发血和尿样中氟乙酰胺鼠药的GC/MS定量分析新方法 ,并用于实际案例检测。方法 选择乙酰胺为内标 ,通过比较不同固相柱的萃取效率和不同条件对回收率的影响 ,优化用于血和尿样中氟乙酰胺萃取的固相柱和提取条件 ,利用氟乙酰胺与乙酰胺质谱图的分子离子峰面积之比与氟乙酰胺浓度的定量关系 ,建立血和尿样中氟乙酰胺鼠药的GC/MS定量分析新方法。结果 用硅胶柱萃取 ,峰面积之比与氟乙酰胺浓度在 5 0~ 90 μg/ml范围呈线性关系 ,检测限为 1 0 μg/ml。血样中氟乙酰胺检测的平均回收率达 91 6% ,标准偏差小于 7 3 %。结论 此法对实际样品的测定证明可满足氟乙酰胺鼠药中毒的定性定量要求。 相似文献
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腐败生物样品中抗凝血类杀鼠药的HPLC分析研究 总被引:2,自引:0,他引:2
介绍以氯敌鼠、华法令为代表的五种抗凝血杀鼠药的HPLC定性定量分析方法.在酸性条件下液-液提取和C_(18)柱固相萃取方法处理生物样品;选用C_(18)分离柱,流动相分别为:水、乙腈,邻酸二氢钾缓冲液(pH7.0)和甲醇/0.8%醋酸,均做梯度洗脱,DAD检测器,检测波长285nm,外标定量,测得血和肝中的提取回收率>60%.在0.01ug-1.0mg/ml范围内呈现良好的线性关系.适用于腐败生物样品抗凝血类杀鼠药中毒案件的检验及有关临床监测. 相似文献
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Simultaneous Determination of 13 Anticoagulant Rodenticidesin Human Blood by Liquid Chromatography–Tandem Mass Spectrometry and its Application in Three Poisoning Cases 下载免费PDF全文
Zheng Qiao M.Sc. Ping Xiang Ph.D. Baohua Shen M.Sc. Min Shen M.Sc. Hui Yan Ph.D. 《Journal of forensic sciences》2018,63(3):784-792
Anticoagulant rodenticides are widely used for rodent control around the world. A rapid and sensitive method was developed and validated for the simultaneous determination of 13 anticoagulant rodenticides (coumafuryl, pindone, valone, warfarin, coumatetralyl, coumachlor, diphacinone, dicumarol, chlorophacinone, bromadiolone, difenacoum, flocoumafen, and brodifacoum) in human blood by liquid chromatography–tandem mass spectrometry. After liquid–liquid extraction, the anticoagulant rodenticides were separated on an Eclipse Plus C18 column. Linearities were observed for each analyte in blood ranging from 0.5 to 50 ng/mL, with correlation coefficients over 0.99. The limits of detection ranged from 0.01 to 0.2 ng/mL, and the limits of quantification were 0.5 ng/mL for all analytes. The intraday and interday precisions were <15%, and accuracies ranged from 80.3% to 111.0%. This validated method with high sensitivity has been applied in three anticoagulant rodenticide poisoning cases and has been used successfully in monitoring blood concentrations for months. 相似文献
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目的建立尿样和头发中甲基苯丙胺的基质辅助激光解吸飞行时间质谱(matrix-assisted laser desorption/ionization time of flight mass spectrometry,MALDI-TOF-MS)分析方法。方法尿样采用液液提取,头发经0.1mol/L盐酸水解后采用液液提取,以碳纳米管为基质应用MALDI-TOF-MS法检测。结果尿样中甲基苯丙胺的最低检测限(LOD)为0.5μg/mL,线线范围为线性范围为0.5~100μg/mL(R2=0.9970);毛发中甲基苯丙胺的最低检测限(LOD)为0.4ng/mg,线性范围为0.4~60ng/mg(R2=0.9976),对送检案例中尿样和头发检材进行检测,效果良好。结论本方法适用于尿样和头发中甲基苯丙胺的分析,与传统气相色谱质谱联用和液相色谱-质谱联用相比,分析速度更快,适合大批量样品同时分析。 相似文献
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尿中香豆素类抗凝血杀鼠剂的固相萃取-紫外导数光谱测定 总被引:1,自引:0,他引:1
尿中杀鼠灵、杀鼠迷、溴敌隆、大隆等4种杀鼠剂用GDX403大孔树脂吸附,二氯乙烷洗脱。通过洗脱液二阶导数光谱,测定杀鼠剂含量。4种杀鼠剂尿中回收率分别为96.3±4.1%、95.6±3.3%、 85.2±4.0%、77.5±3.6%(mean±S.D),检出限分别为0.6、0.6、1.0、1.0mg/L。适用于司法毒物分析。 相似文献
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To validate information on cannabis use, we investigated human hair and pubic hair for cannabinoids (THC and THC-COOH) by gas chromatography/mass spectrometry. Samples (100 mg approximately) were decontaminated with methylene chloride, then pulverized and dissolved in 1 ml 1 N NaOH for 10 min at 95 °C in the presence of 200 ng of deuterated standards. After cooling, samples were extracted by n-hexane/ethyl acetate after acidification with acetic acid. After derivatization of the dry extract by PFPA/PFP-OH, the drugs were separated on a 30-m capillary column and detected using selected-ion monitoring (m/z 377 and 459 for THC and THC-COOH, respectively). Forty-three hair samples were obtained from fatal heroin overdose cases. Among them, 35% tested positive for cannabinoids. Hair concentrations ranged from 0.26 to 2.17 ng/mg (mean, 0.74 ng/mg) and 0.07 to 0.33 ng/mg (mean, 0.16 ng/mg) of THC and THC-COOH, respectively. As is generally the case for other drugs detected in hair, metabolite concentration was always lower when compared to the parent drug concentration. In pubic hair, THC concentrations ranged from 0.34 to 3.91 ng/mg (mean, 1.35 ng/mg) and THC-COOH concentrations from 0.07 to 0.83 ng/mg (mean, 0.28 ng/mg). In most cases, the highest cannabinoid concentration was found in pubic hair, suggesting that this sample may be the more suitable for cannabis testing. 相似文献
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A 35-year-old male was found lying in a prone position in his room. He was in cardiopulmonary arrest on arrival to hospital and was pronounced dead. There was no attempt at resuscitation. No miosis was observed on admission. At post-mortem his stomach contained 170 g greenish liquid with a small amount of shredded tobacco leaves. The serum cholinesterase activities were 47-90 IU (normal range for male: 200-440 IU). GC and GC-MS analyses showed nicotine (21.8 mg), methomyl (304 mg), and triazolam (1.69 mg) in his stomach. He had consumed tobacco leaves, Lannate containing water soluble methomyl (45%), and Halcion tablets containing 0.25 mg triazolam. Methomyl concentrations in blood were 3-8 ng/ml. Substantial amounts of methomyl (2260-2680 ng/ml) were detected in cerebrospinal fluid and vitreous humor. Nicotine concentrations in blood ranged from 222 to 733 ng/ml. A small amount of triazolam was detected only in bile (176 ng/ml) and liver (23 ng/g). The cause of death was respiratory paralysis produced by the additive effects of methomyl and nicotine shortly after consumption. 相似文献