Quantitative determination of strychnine in blood and urine by gas chromatography with mass-selective detector

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.     

大鼠血液、尿液中阿米替林的气相色谱快速分析

目的建专：m液及尿液中阿米替林（AMTL）的气相色谱分析方法,、方法以正常大鼠m液及尿液为空F1样奉,分别添加AMTI-标准品和内标SKF525A。实验大鼠以AMTL2倍LD50灌胃,致大鼠急性中毒后提取血液及尿液。用乙醚提取样本中AMTL,采用GC／FID法进行定量分析,并考察实验条件,结果采用该方法,血液及尿液中AMTL线性池用分别为5～150μg／mL（r=0．993）和5～150μg／mL（r=0．998）;最低检测限（S／N／〉3）均为1．0陆g／mL;口内、口间精密度均小于6％,同收率存95.5％～105．6％之间。结论该方法方操作便捷、捧确度高,适用=fAMTL临床治疗中血药浓度快速监测和法医毒物分析鉴定。     

Two tricyclic antidepressant poisonings: levels of amitriptyline, nortriptyline and desipramine in post-mortem biological samples

Two deaths due to amitriptyline and desipramine overdoses are reported. The first case deals with a 20-year-old Caucasian male who was found dead at his residence. Toxicological analysis of the blood, urine, liver and kidney revealed the presence of amitriptyline (1.7 mg/l, 0.13 mg/l, 36.0 mg/kg and 98.0 mg/kg) and nortriptyline (0.66 mg/l, 0.74 mg/l, 12.0 mg/kg and 37.0 mg/kg). The gastric content contained only 220 mg of amitriptyline. The urine also contained norverapamil, which was consistent with previous verapamil therapy. The second case involved a 19-year-old Caucasian male who attempted suicide earlier and was on desipramine medication. The blood, urine, liver and gastric content disclosed the presence of desipramine in the concentrations of 14.2 mg/l, 33.7 mg/l, 112.5 mg/kg and 180 mg, respectively. The levels of these tricyclics analyzed by high pressure liquid chromatography were in agreement with the levels reported in the literature. Though with the amitriptyline poisoning no significant anatomic changes were noted, the desipramine-caused death was further supported by the multisystem vascular congestion and ischemic changes consistent with cardiopulmonary failure.     

Determination of carbon monoxide in blood by gas chromatography using a thermal conductivity detector

A method is described for the gas chromatographic quantitation of carbon monoxide by means of thermal conductivity detection. Carbon monoxide is released from blood samples as small as 0.02 mL using a unique extraction chamber. The method was compared to a standard gas chromatographic and spectrophotometric method of carbon monoxide quantitation. It was comparable to the former with all samples evaluated and apparently more reliable than the latter with decomposed samples.     

The detection of isoniazide in the cadaveric blood and plasma by high performance liquid chromatography with a diode matrix detector

The authors describe the analytical procedure for the rapid detection of isoniazide in the cadaveric blood and plasma using high performance liquid chromatography with a diode matrix detector (HPLC-DAD). The method is designed for toxicological and forensic medical analyses. The preliminary preparation of the samples includes protein precipitation with trichloroacetic acid, formation of isoniazide derivatives with cinnamic aldehyde, and chromatographic analysis on an Eclipse XDB-C18 column with registration of absorption at a wavelength of 340 nm. The mobile phase is a mixture of methanol and 0.05 M ammonium acetate buffer (50:50 v/v), pH 3.8. The detection limit is 0.5 mcg/ml in plasma and 1 mcg/ml in blood hemolizate. The qualitative determination is possible in a concentration range from 2 to 200 mcg/ml. Mean square deviation does not exceed 12% in a concentration interval from 2 to 50 mcg/ml.     

Gas chromatography in quantitative analysis of hydrocyanic acid and its salts in cadaveric blood

A direct gas chromatography method was designed for the quantitative determination of cyanides (prussic acid) in cadaveric blood. Its sensitivity is 0.05 mg/ml. The routine volatile products, including substances, which emerge due to putrefaction of organic matters, do not affect the accuracy and reproducibility of the method; the exception is H-propanol that was used as the internal standard. The method was used in legal chemical expertise related with acute cyanide poisoning (suicide) as well as with poisoning of products of combustion of nonmetals (foam-rubber). The absolute error does not exceed 10% with a mean quadratic deviation of 0.0029-0.0033 mg.     

SPE—GC／MS、GC／NPD法检测血液中苯丙胺类毒品

目的利用GC／MS、GC／NPD与固相萃取（SPE）技术相结合,建立血液中苯丙胺类毒品的定性定量分析方法。方法采用Bond—ElutCerti{y固相柱、甲醇淋洗、二氯甲烷／异丙醇／氨水（78／20／2）洗脱固相萃取分离提取,比较了不同PH体系、稀释状态、洗脱溶剂对提取回收率的影响,建立血液中苯丙胺类毒品的GC／MS、GC／NPD定性定量分析方法。结果以GC／NPD分析AM、MA、MDA和MDMA浓度在15ng／mL-2000ng／mL、10ng／mL～1600ng／mL、20ng／mL-3000ng／ml、20ng／mL-3000ng／mL范围内线性关系良好,AM、MA、MDA和MDMA的检测限分别为10ng／mL、8ng／mL、15ng／mL、15ng／mL,方法平均回收率大于85％,标准偏差小于5％,GC／MS-Scan检测限分别为40ng／mL、32．0ng／mL、60．0ng／mL、60．0ng／mL。结论此方法可满足苯丙胺类毒品滥用者的血液定性定量分析。     

Detection of amitriptyline, nortriptyline and bromazepam in liver, CSF and hair in the homicidal poisoning of a one-month-old girl autopsied 8 months after death

We reported on the death by poisoning of a one-month-old baby that had followed the death of one of her sister (due to cyamemazine overdose). Exhumation of the corpse was done 8 months after burial and revealed the presence of amitriptyline. Parent drug and its metabolite were analysed by HPLC-MS/MS in positive ionisation mode on a C(18) analytical column using a gradient of acetonitrile and 2mM formate buffer at pH=3. Quantification is based on the main ion m/z=233, the common product ion of nortriptyline (MH(+), m/z 264), amitriptyline (MH(+), m/z 278) and nortriptyline D3 used as internal standard (MH(+), m/z 267). Amitriptyline and nortriptyline in the liver were measured at a concentration of 29.8 and 3.6 μg/g, respectively. Hair analyses revealed the presence of amitriptyline and nortriptyline at concentrations of 1811 and 43 pg/mg, respectively, while complementary analyses showed the presence of bromazepam in the hair at a concentration of 740 pg/mg, thus documenting previous administrations. The mother confessed later having used the drinkable form of the pharmaceutical LAROXYL(?) by pouring the content of a 20 ml bottle (at 40 mg/ml) into the feeding-bottle of her child. The milk was sweet but still bitter and following the testimony of a close relative, the whole family helped to feed the crying baby.     

Analysis of clonidine in biological fluids using gas chromatography with an electron capture detector

The method of clonidine identification in blood and urine is described. It is based on liquid-liquid extraction and purification with toluol, subsequent derivation with pentafluobenzoylchloride and test on gas chromatograph with a detector of electron capture. The method is proposed for expert examinations.     

GC双检测器技术筛选常见毒(药)物的可行性研究

利用气相色谱仪 ,在样品进样经单柱分离后通过Y形管连接至两个不同选择性检测器 (NPD/FID)的方法 ,考察气相色谱操作条件对双检测器响应比值的影响及其该法用于复杂样品测定的可行性。结果表明当实验条件保持不变时 ,NPD/FID响应比值具有较好的重现性。改变检测器操作参数和色谱条件对NPD/FID响应比值都有影响 ,但相对于某一参比物计算得到的相对NPD/FID响应比值受影响很小。样品中待测组份的浓度改变不影响NPD/FID响应比值。在有标准品比对的情况下 ,NPD/FID响应比值或相对NPD/FID响应比值可以作为定性分析的一个参数。     

便携式血液中CO检测仪的研制与应用研究

目的 依据分光光度计还原法原理,利用微型锂电池、传感器、全分析系统,研制特定波长便携式血液中CO检测仪.方法 选择以发光二极管(LED)为光源的单光源模式,以比色皿为样品池,设置内部参比,对光强进行校正.整个系统进行集成,实现数据采集、信号处理和运算一体化,直接显示测定结果.结果 最终形成体积小、质量轻、操作简便、检测...     

GC/MS、GC/NPD法检测血液中氯胺酮

目的利用GC/MS、GC/NPD与固相萃取（SPE）技术相结合,建立血液中氯胺酮的定性定量分析方法。方法选择4-苯基丁胺为内标,采用Bond-Elut Certify固相柱萃取、二氯甲烷：异丙醇：氨水（78∶20∶2,v/v/v）洗脱的固相萃取分离技术,比较不同pH体系、洗脱溶剂对回收率的影响,建立血液中氯胺酮的GC/MS、GC/NPD定性定量分析方法。结果以GC/NPD分析氯胺酮在6.0～5000ng/mL范围内线性关系良好,GC/MS-Scan定性检测限为20.0ng/mL。方法平均回收率达96.9%,标准偏差小于5%。结论此方法可满足氯胺酮毒品滥用者血液定性定量分析。     

GC/MS、GC/NPD法检测毛发中的氯胺酮

目的采用液-液萃取、衍生化和GC/MS、GC/NPD方法,进行毛发中氯胺酮定性定量分析。方法选择4-苯基丁胺为内标,毛发样本用NaOH、HCl及芳基硫酸酯酶/β-葡萄糖醛酸酶等3种方式进行水解,再进行衍生化后,采用GC/MS和GC/NPD方法定性定量分析。对不同水解和衍生化条件以及提取溶剂进行比较优化,并考察方法精密度、稳定性和检出限。结果方法的提取回收率大于95%,精密度和样品稳定性良好,日内和日间标准偏差小于6%;采用GC/NPD和GC/MS直接分析毛发中的氯胺酮,检出限为0.2ng/mg和2.0ng/mg,线性范围为10.0～250.0ng/mg,相关系数均大于0.99;采用酰化衍生化后分析,GC/NPD和GC/MS检出限分别提高至0.1ng/mg和0.2ng/mg。结论该方法回收率高、检测限低,可以用于毛发中氯胺酮的定性定量分析检验。     

直接进样气相色谱法测定全血中乙醇的含量

目的建立一种直接进样气相色谱法检测全血中的乙醇。方法全血经硫酸铝钾沉淀蛋白,加入内标异丙醇后,用直接进样气相色谱法进行检测,FID为检测器,用保留时间定性,内标标准曲线法定量。结果该方法线性范围为0.2-1.4mg/m L,相关系数R=0.999 3,总分析时间不超过5min,最低检测限为0.01mg/m L,相对标准偏差（RSD）〈5%,平均回收率为92.3%;所建立的方法与顶空气相色谱（HS-GC）法比较相对偏差（RD）〈10%。结论该方法可用于全血中乙醇的检测。     

Chemico-toxicological analysis of haloperidol in blood with high-performance liquid chromatography in combined poisoning

Haloperidol is widely used in psychiatric practice both in monotherapy and in combination with neuroleptics, phenothiazine derivatives (chlorpromasin, levomepromasin) and antidepressants (amitriptilin, imipramin). We have developed techniques of haloperidol isolation from blood in combined poisonings with phenothiazine derivatives (chlorpromazine, levomepromasine) and antidepressants (amitriptilin, imipramin), their identification and quantitation with high-performance liquid chromatography. The highest output of the substances studied was achieved in alkaline hydrolysis. The techniques are expressive, sensitive and well reproducible. This makes them convenient for practice of forensic-chemical and chemico-toxicological laboratories.