气相色谱法测定复方冰片搽剂中冰片、薄荷脑和樟脑的含量

目的：建立复方冰片搽剂中冰片、薄荷脑和樟脑的含量测定方法。方法：采用气相色谱法，色谱柱：10％PEG-30M石英毛细管色谱柱；柱温：150℃；进样口温度250℃；程序升温；FID检测器。结果：冰片、樟脑和薄荷脑平均回收率分别为：99．6％（RSD为0．8％）、99．8％（RSD为0．9％）、98．5％（RSD为1．0％）。结论：本法简便准确灵敏，可用于本品的质量控制。     

GC—MS定性定量分析生物检材中的安眠酮

目的：建立定性定量检测人体尿液、血液及唾液中安眠酮的分析方法。方法：尿液、血液、唾液等生物样本中的安眠酮经固相萃取法进行提取后,用气相色谱-质谱仪进行定性定量分析,从线性、抗干扰性、精密度、回收率及稳定性等方面对方法进行验证。结果：安眠酮浓度在0—400．0ng·mL^-1的范围内线性良好（r≥0．999）,方法的最低检出量为8．0ng·mL^-1;最低定量限为100．0ng·mL^-1;方法的日内、日间精密度CV≤5％（n=6）;各基质中前处理回收率在±10．0％（n=3）范围内。结论：本方法检测准确、灵敏、特异性好,可满足尿液、血液、唾液等生物检材中安眠酮的定性定量分析。     

固相萃取-气相色谱质谱法测定生物材料中的氯氮平

目的：建立氯氮平的固相萃取．气相色谱质谱(SPE-GC-MS)测定法。方法：血液及肝中的氯氮平用固相萃取柱分离后，以SKF525A为内标，用气相色谱质谱法测定其含量，同时对该法的检测限、线性范围及回收率进行探讨。结果：氯氮平的检测限为0．05ng，线性范围为0．5～100ng，血中平均回收率为90．1％，RSD为8．3％(n=6)。结论：本法检验并测定生物材料中的氯氮平，操作简便，结果准确，重现性好。     

气相色谱顶空进样法检测盐酸林可霉素中有机溶剂残留量

目的采用气相色谱顶空进样法检测盐酸林可霉素原料药中的有机溶剂丙酮、丁醇残留量。方法采用DB-624毛细管色谱柱（30m×0．53mm，3um），程序升温，采用FID检测器，载气为氮气。结果丙酮、丁醇完全分离，其质量浓度分别在8．0～119．4ug／mL、10．0～120．6ug／mL范围内与峰面积呈良好的线性关系，相关系数分别为0．9993和0．9995，平均回收率分别为102．9％（RSD=2．4％），102．3％（RSD=1．9％）：最低检测限分别为2ug／mL和2．5ug／mL，精密度RSD均小于5％。结论本试验建立的方法简便灵敏，结果准确可靠，适用于盐酸林可霉素中有机溶剂残留量的检测。     

顶空气相色谱法测定头孢泊肟酯中有机溶剂残留量

目的：建立头孢泊肟酯中8种有机溶剂残留量的分离测定方法。方法：采用顶空进样毛细管气相色谱法，程序升温，正丁醇为内标，N，N-二甲基甲酰胺为溶解介质，色谱柱为DB-624毛细管柱，载气为氮气，FID检测器，测定了头孢泊肟酯原料药中甲醇、丙酮、二氯甲烷、异丙醚、乙酸乙酯、四氢呋喃、甲苯、乙酸丁酯的残留量。结果：8种有机溶剂完全分离，在所考察的浓度范围内具有良好线性，r为0．9945～0．9996，平均回收率82．02％～107．9％，精密度、重复性RSD均小于5%。结论：本实验建立的色谱方法灵敏、准确，适用于头孢泊肟酯中有机溶剂残留量的检测。     

毛细管GC测定石杉碱甲贴片中有机溶剂残留量

目的：建立石杉碱甲贴片中异丙醇、乙酸乙酯残留量的测定方法。方法：采用毛细管气相色谱法，色谱柱为HP-5（5％二苯基-95％二甲基聚硅氧烷）；柱温：40℃。载气为氮气；检测器为FID；外标法计算含量。结果：在该色谱条件下，测得乙酸乙酯和异丙醇两溶剂在2．50—12．5μg-mL^-1范围内线性均良好（r=0．9991和0．9994）；平均回收率分别为96．57％和98．09％，RSD分别为1．4％和1．7％；异丙醇、乙酸乙酯的最低检测限均为0．5ng；10批样品中上述有机溶剂残留量均符合ICH和GMP要求。结论：该毛细管气相色谱法灵敏、准确、可靠，适用于本品中有机溶剂残留量测定。关键词：石杉碱甲；贴片；毛细管气相色谱法；有机溶剂残留量     

气相色谱法测定冠心苏合口腔崩解片中土木香内酯含量

目的建立气相色谱法测定冠心苏舍口腔崩解片中土木香的含量。方法采用DB-1毛细管色谱柱，FID检测器，程序升温，初始温度150℃，以每分钟5℃升温至220℃，再以每分钟50℃升温至260℃，保持6min。结果土木香内酯质量浓度的线性范围为22—221μg／mL（r=0．9999），平均回收率为97．2％，RSD=1．5％（n=6）。结论气相色谱法灵敏、准确、可靠，可作为冠心苏合口腔崩解片的质量控制方法。     

基于HPLC法测定血浆中氟哌啶醇浓度

目的建立高效液相色谱（HPLC）法测定血浆中氟哌啶醇浓度的方法。方法以乙腈-甲醇-0．025mol／L磷酸二氢钾（45：5：50,v／v）为流动相,氯氟哌啶醇作内标,紫外波长248nm处检测。结果血浆中氟哌啶醇的最低检测浓度为0．5ng／ml,平均提取回收率为86．7％±5．0％,线性范围1～50ng／ml（r=0．9998）,日内和日间RSD分别小于8％和9％。结论方法灵敏、快速、准确,可满足临床治疗药物的监测工作。     

HPLC法测定血清中全反式维甲酸浓度

目的 为了检测体内全反式维甲酸浓度及其药物动力学研究的需要。建立了血清全反式维甲酸的反相高效液相色谱(HPLC)的分析方法。方法 血液离心后取上清加丙酮、乙醚，离心后取上清有机层，真空提取干燥后用甲醇溶解后采用HPLC进行检测分析。结果 该方法的THP最低检出浓度为1．4ng／ml血液标本浓度在0．1-1000ng／ml间具有良好的线性关系，r≥0．997，回收率91．2％-97．2％变异系数，批内2．8％-6．2％，批间3．1％-11．8％。结论 该方法灵敏、快速、准确、重复系数好。     

毛细管气相色谱法检测生长抑素中有机溶剂残留量

目的：建立生长抑素中4种有机溶剂残留量的分离测定方法。方法：采用直接进样毛细管气相色谱法，程序升温，色谱柱为DB-624毛细管柱，载气为氮气，FID检测器，双蒸水为溶解介质，检测了生长抑素原料药中乙腈、哌啶、醋酸、Ⅳ，Ⅳ-二甲基甲酰胺的残留量。结果：4种有机溶剂完全分离，在所考察的浓度范围内具有良好线性，r为0．9997—1．000，乙腈、哌啶、醋酸、Ⅳ，Ⅳ-二甲基甲酰胺的检测限分别为0．3，2．2，1．3，0．4ng，精密度RSD均小于5％，平均回收率为103．3％-105．6％。结论：本试验建立的方法简便灵敏，结果准确可靠，适用于生长抑素中有机溶剂残留量的检测。     

Determination of p-tert-octylphenol in blood and tissues by gas chromatography coupled with mass spectrometry

A sensitive and reproducible procedure using gas chromatography coupled with mass spectrometry is described for the determination of p-tert-octylphenol (OP), a persistent degradation product of alkylphenol ethoxylates that binds to the estrogen receptor in blood and tissues. The first step involved the extraction of blood (200 microL) or tissue homogenate (400 microL) with methyl tert-butyl ether, including p-tert-butylphenol (BP) as internal standard. After extraction, the sample was evaporated to dryness with a gentle stream of nitrogen at 45 degrees C, and OP and BP were derivatized with an acetylation reaction involving acetic anhydride and catalyzed by pyridine. Samples were then analyzed by a gas chromatograph equipped with a mass spectrometer (single ion monitoring) with a Varian VF-5ms capillary column. The limit of detection and the limit of quantification of the method in blood were 4.6 and 15.5 ng/mL, respectively. The linearity and reproducibility of the method were acceptable, with coefficients of variation of approximately 10% for blood and ranging between 9% and 27% for tissues. This method was applied to the determination of unchanged OP in blood and tissues obtained from Sprague-Dawley rats after oral and IV OP administration.     

delta-9-Tetrahydrocannabinol analysis in forensic blood specimens using capillary column gas chromatography with nitrogen sensitive detection

A method for the determination of delta-9-tetrahydrocannabinol (THC) in whole blood that employs hexane extraction followed by identification using gas chromatography with nitrogen/phosphorus detection has been developed. The assay is sensitive to 2 ng THC per mL blood and linear to concentrations up to 120 ng/mL (r = 0.998). Precision is demonstrated by coefficients of variation ranging from 3.6 to 9.1% (within run) and 7.1 to 8.0% (between run).     

Methodology for the determination of dinitroaniline herbicides in tissue and excreta

A method is presented for the analysis of trace amounts of dinitroaniline herbicides in tissue and excreta. The method employs extraction of the tissue or excreta with organic solvent, clean up by liquid/liquid partitioning or silica gel chromatography, and ultimate analysis by gas chromatography using electron capture detection. Recoveries of greater than 80% were noted over the range of concentration 0.1 to 1.0 microgram/g.     

Automated solid-phase extraction method for the determination of piperaquine in whole blood by rapid liquid chromatography

A bioanalytic method for the determination of piperaquine in whole blood by solid-phase extraction and rapid liquid chromatography has been developed and validated. Whole blood was hemolyzed with deionized water, and an internal standard was added to the samples before they were loaded onto a PRS cation-exchange solid-phase extraction column. Piperaquine and internal standard were analyzed by liquid chromatography on a Chromolith Performance (100 x 4.6 mm) column with mobile phase acetonitrile:phosphate buffer, I = 0.1, pH 2.5 (8:92, vol/vol), flow rate 4 mL x min-1, and UV detection at 345 nm. The intraassay precision for whole blood was 3.2% at 3.00 microM and 12.3% at 0.100 microM. The interassay precision for whole blood was 1.8% at 3.00 microM and 5.2% at 0.100 microM. The lower limit of quantification and the limit of detection were 0.050 microM and 0.010 microM, respectively.     

Rapid analysis of halothane in biological samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry--a case of a double homicide

A simple, rapid, and sensitive method for the analysis of halothane in biological samples was developed. The procedure describes the extraction of halothane from blood, liver, kidney, brain, urine, bile, and stomach contents by headspace solid-phase microextraction (HS-SPME) followed by capillary gas chromatography coupled with mass spectrometry (GC-MS). The recovery in blood samples after addition of ammonium sulfate and sulfuric acid was 72% compared to a sample prepared in water (100%). Linearity was established over a concentration range of 0.1-100 mg/kg of spiked blood samples with an excellent coefficient of correlation (0.996) and a limit of detection of 0.004 mg/kg. The time for analysis was approximately 40 min per sample including the extraction step. The procedure was used for quantitation of halothane in various samples in a case of a double homicide. HS-SPME in combination with GC-MS was an effective method for the determination and quantitation of halothane in biological material.     

Confirmation of a carboxylic acid metabolite of polychlorotrifluoroethylene and a method for its GC-ECD analysis in biological matrices.

3.1 Oil, referred to as polychlorotrifluoroethylene (pCTFE), is a polymeric mixture consisting primarily of trimers and tetramers of chlorotrifluoroethylene (CTFE) end-capped with chlorine. Inhalation studies have associated dose-related body weight loss, increased organ weights, and abnormal hepatic enzyme activities with exposure to pCTFE. The carboxylic acid metabolites of pCTFE have been shown to cause hepatotoxicity in rats, which is manifested by increased liver weights and the proliferation of hepatic peroxisomes. A method was developed to derivatize these carboxylic acid metabolites. Tissue homogenates and feces were extracted with methanol, and urinary metabolites were extracted on octadecylsilane (ODS) solid-phase extraction columns. Aliquots of the extracts and whole blood were methylated with 3N methanolic HCl to transesterify the carboxylic acid metabolites to volatile methyl esters. The pCTFE methyl esters were analyzed by gas chromatography (GC) with electron capture detection (ECD). The on-column limit of detection was 5 pg for each methyl ester. Solid-phase extraction of spiked urine gave extraction efficiencies of 90.4% for the trimer acid and 84.7% for the tetramer acid. This method was successfully applied to toxicity studies in rats and nonhuman primates. The identities of the derivatized metabolites were confirmed by GC/MS.     

Simultaneous congener-specific determination of selected organochlorine compounds and nitro musks in human whole blood samples by solid-phase extraction and capillary gas chromatography with electron capture detection

Chlororganic compounds like pesticides or polychlorinated biphenyls (PCB) and nitro musks are environmental contaminants, which remain public health concerns because of their persistence in humans and their toxicological properties. Many of these substances are associated with endocrine dysfunction or with carcinogenicity. Therefore, a simple method using solid-phase extraction followed by capillary gas chromatography with electron capture detection for the simultaneous determination of both organochlorines and nitro musks in human whole blood samples has been developed. Recovery rates of 13 PCB congeners and of 7 pesticides ranged from 67.5% to 100.4% and from 81.1% to 110.5%, respectively. Recoveries of the 5 nitro musks were consistent and ranged from 90.2% to 98.8%. The accuracy for organochlorines and nitro musks varied from 6.3% to 8.6%. Method detection limits ranged from 0.02 microg/L to 0.11 microg/L for the organochlorines and from 0.04 microg/L to 0.08 microg/L for the nitro musks. The method has a high sensitivity with a low detection limit even in slightly contaminated human blood samples. The time and technical effort is small, so the method is feasible for epidemiological studies with regard to the impact of organochlorines and nitro musks on certain diseases.     

Headspace solid-phase micro-extraction and gas chromatography with micro-electron capture detection for the measurement of p,p'-DDE in rat whole blood and hair

A sensitive, specific, and reproducible capillary gas chromatography (GC) with micro-electron capture detection (micro-ECD) method using headspace solid-phase micro-extraction (HS-SPME) for the quantitative analysis of p,p'-DDE in rat whole blood and hair was developed. A 100 microm polydimethylsiloxane (PDMS) phase was used for the extraction. The obtained detection limits were 0.003 ng/mg and 0.004 ng/mg in whole blood and hair, respectively, at a signal-to-noise ratio of 3 (S/N = 3). Linearity was obtained in the ranges 0.003-2.0 ng/mg and 0.004-2.0 ng/mg in whole blood and hair, respectively, and the correlation coefficients of whole blood and hair were greater than 0.998. This method was successfully applied to the analysis of p,p'-DDE in rat whole blood and rat hair after an oral dose of p,p'-DDE.     

A comparison of a commercial microdiffusion method and gas chromatography for ethanol analysis

A simple, rapid ethanol screen based on a microdiffusion technique (Toxi-Lab alcohol test) was evaluated using whole blood and urine samples and compared to a direct injection gas chromatographic technique. A total of 204 samples were analyzed, 124 whole blood specimens and 80 urine samples. The whole blood samples showed agreement in 79 of 80 samples that tested positive by gas chromatography. All 44 whole blood samples that tested negative by gas chromatography were also negative by the microdiffusion method. All urine samples, both positive and negative, as well as all control specimens showed agreement. The one whole blood sample that did not agree had an ethanol level by gas chromatography below the stated detection limit (0.01%) of the microdiffusion method. The microdiffusion method was found to be a viable screening test for the presence of ethanol in whole blood and urine. It is relatively inexpensive and rapid and is therefore an ideal method for screening samples before a more expensive or time-consuming confirmatory method.     

The determination of delta9-tetrahydrocannabinol and 11-nor-9-carboxy-delta9-tetrahydrocannabinol in whole blood using solvent extraction combined with polar solid-phase extraction

A method for the determination of delta9-tetrahydrocannabinol (THC) and 11-nor-9-carboxy-delta9-tetrahydrocannabinol (THCCOOH) in whole blood using conventional solvent extraction followed by a cleanup using polar solid-phase cartridges is described. The method uses 0.5 mL of blood, and detection is by benchtop gas chromatography-mass selective detection using selected ion monitoring. The limit of detection is better than 1 ng/mL, and extraction efficiencies are greater than 80% for THC and 70% for THCCOOH. The method is robust and highly reproducible.