Rapid isolation with Sep-Pak C18 cartridges and wide-bore capillary gas chromatography of some butyrophenones

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.     

尿液中几种碱性麻醉药物的检验

本文介绍了一种用 Sep-Pak C_(18)小柱,液-固萃取法提取尿液中几种碱性麻醉药物,以大口径毛细管气相色谱-氢火焰离子化检测器检验的方法。操作过程简单、迅速,各药物回收率高。     

Rapid isolation of benzodiazepines with Sep-Pak C18 cartridges

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.     

Positive and negative ion mass spectrometry and rapid isolation with Sep-Pak C18 cartridges of ten local anaesthetics.

The positive ion electron impact (PIEI), positive ion chemical ionization (PICI) and negative ion chemical ionization (NICI) mass spectra and a rapid isolation procedure using Sep-Pak C18 cartridges are presented for ten local anaesthetics. In the PIEI mode, molecular peaks were very small or missing for most compounds. Peaks at m/z 86 due to the diethylaminoethyl or propylaminoethyl group constituted base peaks in six compounds. In the PICI mode, peaks due to M + H and M + C2H5 appeared. The cation at m/z 86 was also observed for the six compounds. This ion seems useful for the screening of local anaesthetics. In the NICI mode, anions at m/z M - H constituted base peaks for all compounds, peaks at m/z M + 12 appeared in many compounds. The total ion current in the PIEI and PICI modes generally gave higher sensitivity than in the NICI mode. Local anaesthetics present in whole blood or cerebrospinal fluid (CSF) could be rapidly isolated by use of Sep-Pak C18 cartridges with chloroform/methanol as an elution solvent. Their detection was possible using wide-bore capillary gas chromatography with SPB-1 and HP-17 wide-bore capillary columns with satisfactory separation from impurities.     

Solid phase extraction method for rapid isolation and clean-up of some synthetic pyrethroid insecticides from human urine and plasma.

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.     

Rapid isolation with Sep-Pak C18 cartridges and capillary gas chromatography of triazine herbicides in human body fluids.

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.     

用Sep—Pak C18固相萃取柱快速提取净化氨基甲酸酯类农药

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。     

Rapid extraction and capillary gas chromatography for diazine herbicides in human body fluids

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.     

Positive- and negative-ion mass spectrometry and rapid clean-up of some carbamate pesticides

Positive-ion electron impact (PIEI), positive-ion chemical ionization (PICI) and negative-ion chemical ionization (NICI) mass spectra of 9 carbamate pesticides are presented. In the PIEI mode, the spectra showed small molecular peaks, intense or base peaks due to M - CH3NHCO + H and peaks at m/z 58 due to CH3NHCO. In the PICI mode, peaks due to M + H, M + C2H5, M - CH3NHCO + 2H, CH3NHCO(m/z 58) and M-28 appeared. The cations at m/z 58 found in both PIEI and PICI modes seem very useful for screening of a carbamate. In the NICI mode, the spectra showed peaks due to M - CH3NHCO and characteristic anions appearing at mass numbers higher than molecular ones, which were probably due to dimerization of [M - CH3NHCO]-followed by hydrogen attachment. Carbamates, which had been added to urine, plasma, whole blood, the liver, kidney and brain, could be rapidly isolated by use of Sep-Pak C18 cartridges with chloroform as an elution solvent. They could be detected by wide-bore capillary gas chromatography with a SPB-5 column, with satisfactory separation from impurities in their underivatized forms.     

Wide-bore capillary column gas chromatography in toxicological analysis of biological samples from multidrug overdoses fatalities

Fatalities from multidrug overdoses account for 25% of the total number of all poisoning fatalities and as such deserve greater attention from researchers than single drug overdoses. High resolution, good sensitivity, and repeatability provided by gas chromatography (GC) with wide-bore capillary silica and glass columns make GC particularly useful for identification and quantitative analysis of drugs in toxicological screening of autopsy specimens. Results of toxicological findings in three deaths from multidrug overdoses (methaqualone, doxepine, methotrimeprazine, pernazine-aspirin, paracetamol, codeine-morphine, diazepam) occurring in routine medical practice are reported.     

用固相萃取法提取净化生物检材中拟除虫菊酯类杀虫剂的实验研究

固相萃取法（Sep－PakC18小柱）同时萃取净化生物检材（血浆、尿）中的甲醚菊酯、灭扫利、功夫、二氯苯醚菊酯、安绿宝、速灭杀丁和敌杀死。通过气相色谱氢焰检测器、非极性熔融石英大口径毛细管柱及程序升温色谱条件，得到较好的系统分离，并测定萃取回收率在81％～93％（血浆）和90％～102％之间（尿）。实验证明，用70％甲醇稀释检材并用氯仿洗脱可得到较完全的吸附和最佳回收率。     

Rapid isolation of some antiepileptic hydantoins and their analogues with Sep-Pak C18 cartridges and capillary gas chromatography with splitless injection

A simple and rapid method for isolation of seven antiepileptics (2 hydantoin, 2 oxazolidin, and 3 suximide derivatives) from urine and plasma is presented. Urine and plasma (1 ml) samples containing seven antiepileptics were mixed with distilled water (4 ml), and the sample solution was poured into a pretreated Sep-Pak C18 cartridge; this was washed with water and chloroform/methanol was passed through it to elute the antiepileptics. The eluate was mixed with isoamyl acetate and evaporated under a stream of N2. The drugs were detected by gas chromatography with fused silica capillary columns, splitless injection and flame ionization detection. Separation of the seven antiepileptics from each other and from impurities was satisfactory with the use of an SPB-1 capillary column. The detection limit for the seven antiepileptics with the present method was 0.1-1.0 microgram/ml urine or plasma. The recovery of the drugs from urine and plasma was more than 70% and 50%, respectively.     

The application of chromatography and spectrometry for the analysis of ketorolac and diclofenac in biological fluids

The objective of the present work was to study conditions for isolation of ketorolac and diclofenac from biological fluids. A method of their extraction with a mixture of organic solvents has been developed and the conditions for the identification of these compounds are proposed with the use of high performance liquid chromatography (HPLC), UV spectroscopy, and gas chromatography with electron capture detection (GC/ECD). The possibilities of using HPLC, UV spectrometry, and GC/ECD for quantitative determination of ketorolac and diclofenac are illustrated.     

Detection of delta 9-THC in saliva by capillary GC/ECD after marihuana smoking

A method is described for the determination of delta 9-tetrahydrocannabinol (delta 9-THC) in the saliva by the use of a combination of moving-precolumn injector and glass capillary gas chromatograph with electron capture detector (GC/ECD). There were no interfering peaks due to impurities around the peak of pentafluoropropyl derivative of delta 9-THC (delta 9-THC-PFP). This GC/ECD method was linear over the range of 5-200 ng/ml of delta 9-THC-PFP. The lower detection limit was approximately 1 ng/ml. delta 9-THC content in the saliva after experimental marihuana smoking was measured by this method. It was demonstrated that for at least 4 h after smoking the level of delta 9-THC was sufficient for detection.     

毛细管气相色谱法测定酱油中4-甲基咪唑的含量

目的建立毛细管气相色谱法定量分析酱油中有毒成分4-甲基咪唑的方法。方法酱油样品在层析柱中用二氯甲烷洗脱,洗脱液浓缩后加入N,N-二甲基苯胺作为内标,采用DB-FFAP毛细管柱分离样品,氮磷检测器测定4-甲基咪唑含量。结果方法线性范围为4.9~1.5×102μg/L;检测限为0.16μg/L;标准加入0.0102mg和0.0602mg 4-甲基咪唑的平均回收率为97.25%和99.44%。结论本文方法具有操作简便、快速、准确等优点,可用于检验酱油中的4-甲基咪唑。     

Evaluation of the Abbott TDx-radiative energy attenuation (REA) ethanol assay in a study of 1105 forensic whole blood specimens

In a preliminary study to determine the applicability of the Abbott radiative energy attenuation (REA) method for the quantification of ethanol in whole blood specimens it was concluded that a larger number of samples was required to evaluate the method, particularly for use in forensic toxicology applications. In this study, 573 blood specimens from suspected driving while intoxicated individuals (DWI blood) and 532 postmortem blood specimens (PM blood) were analyzed by the REA method and a headspace gas chromatographic method (GC) currently used in this laboratory. "Negative" specimens (less than 10 mg/dL by GC) and "positive" specimens (greater than or equal to 10 mg/dL by GC) in each category were analyzed. Linear regression analysis comparing the REA values with the GC values was performed for each type of blood specimen. The equation obtained for DWI blood specimens was REA = 0.943 GC + 1.54; the equation for PM blood specimens was REA = 0.980 GC + 2.76. The correlation coefficient for each group was greater than 0.99. The data suggested that a limit of detection of 10 mg/dL could be applied for DWI blood specimens, while 20 mg/dL would be recommended as the limit of detection for PM blood specimens.     

Quantitative analysis of tropane alkaloids in biological materials by gas chromatography-mass spectrometry

A simple and rapid method for quantitation of tropane alkaloids in biological materials has been developed using an Extrelut column with gas chromatography-mass spectrometry (GC-MS). Biological materials (serum and urine) were mixed with a borate buffer and then applied to an Extrelut column. The adsorbed tropane alkaloids were eluted with dichloromethane before a GC-MS analysis. Atropine-d(3) was used as an internal standard. The extracted tropane alkaloids were converted to trimethylsilyl derivatives prior to GC analysis, to improve the instability of tropane alkaloids from heating and the property of them for a GC column. The recoveries of the compounds, which had been spiked to biological materials, were more than 80%. The GC separation of the derivatives from endogenous impurities was generally satisfactory with the use of a semi-polar capillary column. Tropane alkaloids showed excellent linearity in the range of 10-5000 ng/ml and the limit of detection was 5.0 ng/ml for biological materials. The present method is simple and more rapid than those previously reported, and was applied to a poisoning case. It is useful for the routine analysis of tropane alkaloids in cases of suspected tropane alkaloids poisoning.     

鸦片中主要成分的检验

本文采用Seppak C_(18)小柱固相萃取鸦片中的五种主要成分,以反相高效液相色谱法,甲醇—甲酸—三乙胺水(35:1.5:0.5:63)为流动相,检验五种成分,各成分均有良好的回收率。方法简单、快速、准确。     

A simple, rapid and simultaneous analysis of complex volatile hydrocarbon mixtures in blood using gas chromatography/mass spectrometry with a wide-bore capillary column

A screening method for detecting volatile hydrocarbons in blood has been developed using gas chromatography/mass spectrometry with a wide-bore capillary column and a headspace method. Toluene-d8 and indan were used as the internal standards for quantitative analysis. Hydrocarbons with retention indices from 600 to 1200 were simultaneously and quantitatively detected in relatively low concentrations (0.01 microgram/ml) in reconstructed ion chromatography. This method could prove useful in forensic cases in which urgent examination of complex hydrocarbon mixtures, e.g. petroleum components, is required.     

Positive- and negative-ion mass spectrometry and rapid clean-up of 19 phenothiazines

Positive-ion electron impact (PIEI), positive-ion chemical ionization (PICI) and negative-ion chemical ionization (NICI) mass spectra of 19 phenothiazines are presented. In the PIEI mode, peaks due to M, M minus side chain (M - R1), M - R1 + H, and side chain itself (R1) appeared for most compounds. The M - R1 and R1 ions were very useful for drug screening. In the PICI mode, most spectra showed base or intense peaks due to M + H, and small peaks due to M + C2H5; peaks due to M - R1 + 2H and R1 also appeared in many compounds. In the NICI mode, fragmentation modes were different in different compound groups; molecular or [M - H]- quasi-molecular anions appeared in many compounds with aliphatic side chains. Anions at m/z 98 and 115 were characteristic for compounds with (N-methylpiperazinyl)propyl side chains. Selected ion monitoring in the PIEI mode generally gave much higher sensitivity than in the PICI and NICI modes. Phenothiazines present in urine or plasma could be rapidly isolated by use of Sep-Pak C18 cartridges. Thirteen of 19 phenothiazines could be detected by HP-17 wide-bore capillary gas chromatography with satisfactory separation from impurities in their underivatized forms.