高效液相色谱/串联质谱法同时测定虾中氯霉素、甲砜霉素和氟甲砜霉素残留量

用高效液相色谱／串联质谱(LC／MS,／MS)同时测定虾中的氯霉素(CAP)、甲砜霉素(TAP)和氟甲砜霉素(FF)。均质后的虾样品,采用碱化乙酸乙酯提取。浓缩提取物经液．液分配(LLP)去除脂肪,C18固相萃取(SPE)柱净化后,采用LC／MS／MS电喷雾电离(ESI),负离子,多反应监测(MRM)模式检测,外标法定量。检出限为：氯霉素和氟甲砜霉素0．01ng/g;甲砜霉素为0．05ng／g。在添加浓度0．1～2．0ng/g范围内,氯霉素回收率为73．9％～96．0％;甲砜霉素回收率为78．6％～99．5％;氟甲砜霉素回收率为74．9％～103．7％;相对标准偏差(RSD)均小于6．4％。     

吹扫捕集-气相色谱分析海水和沉积物中的苯、甲苯、乙苯及二甲苯

单环芳烃苯、甲苯、乙苯和二甲苯（简称BTEX）是石油的重要组分，也是环境中需要重点监测的致癌污染物。本实验建立了动态顶空（吹扫捕集）和光离子化检测器的气相色谱测量海水、沉积物中痕量BTEX的方法。在120—1200ng／L的浓度范围，苯、甲苯、乙苯、间对二甲苯及邻二甲苯标准溶液的检出限分别为6．4、35．2、15．8、12．3、10．7ng／L，相对标准偏差0．9％-6．1％。样品无需预处理，海水中BTEX回收率为93．50％-98．40％。7个渤海表层海水样品中BTEX的浓度均低于140ng／L；海底沉积物中苯、甲苯、乙苯、间对二甲苯及邻二甲苯浓度分别为169—1243、531—1732、1308—5624、237—1136、510—5194ng／L。测量方法和结果对评价环境污染具有重要意义。     

气相色谱法测定空气中苯、甲苯和邻二甲苯

使用3500有机挥发物监控器收集空气中的苯、甲苯和邻二甲苯。建立了气相色谱测定法。方法简单，快速，苯、甲苯和邻二甲苯的检出限小于OSHA允许限量的1／30，回收率为90．8％～99．7％，相对标准偏差为0．40％～0．63％。     

顶空固相微萃取-气相色谱-质谱联用分析纺织品中挥发性有机物

建立了顶空固相微萃取（HSSPME）-气相色谱（GC）-质谱（MS）联用测定纺织品中甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯5种挥发性有机物（VOCs）的分析方法。选择聚二甲基硅氧烷（PDMS）作为萃取涂层，优化了SPME的萃取条件，包括平衡时间、萃取时间、萃取温度、顶空体积、离子强度、搅拌速度、解吸温度和时间以及GC—MS仪器条件。对于甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯方法线性范围分别为0．087～870、3．32～3320、2．28～2280、0．015～150和0．050～50．0ng／g；检出限分别为0．005、0．042、0．670、0．008和0．011ng／g。实际样品加标回收率在80．1％～122％之间，RSD在0．8％～8．6％之间。方法符合纺织品中痕量VOCs的快速分析要求。     

啤酒中N-亚硝胺的SPME-GC-MS分析

研究了固相微萃取-气相色谱-质谱(SPME—GC—MS)联用方法检测啤酒中的N-亚硝基二乙胺(NDEA)、N-亚硝基吡咯烷(NPYR)、N-亚硝基二丁胺(NDBA)，采用聚二甲基硅氧烷／二乙烯苯(PDMS／DVB)萃取头，对影响固相微萃取效率的萃取时间、搅拌速度以及萃取方式等进行了优化，在优化实验条件下，方法的线性范围在12．5～250μg／L之间，相关系数r为0．9971～0．9995，检出限分别为NDEA4．50μg／L，NPYR8．99μg／L，NDBA2．27μg／L，NDBA回收率为86％～96％，相对标准偏差6．296～8．996，该法简化了前处理步骤，快速、方便．结果满意。     

硅胶-氧化铝层析柱-气相色谱法测定沉积物中邻苯二甲酸酯类有机物

建立了硅胶-氧化铝层析柱净化分离,GC—MS、GC—FID定性定量分析沉积物样品邻苯二甲酸酯类有机污染物Phthalate esters（PAEs）的方法。比较了Florisil、硅胶、氧化铝和硅胶-氧化铝层析柱对PAEs分离特征;优化了硅胶-氧化铝层析柱净化分离PAEs的条件。方法线性范围0．05～500μg/g,回收率75.3％～113．6％,相对标准偏差2．74％～12．2％,检出限0．29～1．2ng／g。内标法定量,应用于珠江口沉积物样品中PAEs测定,获得满意的结果。     

高纯金属镱中杂质元素的电感耦合等离子体质谱法测定

利用电感耦合等离子体质谱仪(ICP—MS)直接测定了金属镱中除Tm、Lu外其他稀土及非稀土杂质元素;通过P507萃淋树脂色层柱,分离绝大部分Yb基体,避免了基体元素对Tm、Lu的测定干扰?定量加入内标元素Sc、Cs,有效克服了基体效应所带来的偏差。稀土杂质元素的检出限0．010～0．032μg／g,非稀土杂质元素的检出限为0.12～5．0μg／g。加标回收率为83％～105％。方法适用于纯度为99．99％～99．999％的高纯金属镱产品中杂质元素的测定。     

聚丙烯酸树脂涂层HS-SPME-GC-MS监测城市污水中的芳香烃化合物

采用聚丙烯酸树脂涂层-固相微萃取-气相色谱-质谱(PA—SPME—GC—MS)联用技术,在优化的萃取条件下检测了城市污水中的苯系物和多环芳烃等芳香烃化合物．该方法的最低检出限达12ng／L水平,相对标准偏差为1．7％～9．8％．     

萃取-紫外分光光度法测定微晶蜡中3, 4-苯并芘含量

要采用萃取-紫外吸收光谱法，测定微晶微量3，4-苯并芘的含量．选择二甲亚砜作为萃取溶剂，绘制工作曲线．结果表明，3，4-苯并芘含量在50-3000ng／g的范围内，成良好的线性关系，相关系数为0．9995．检出限为16ng／g．方法重复性好，相对标准偏差为6．2％，回收率在97．0％-99．4％之间．     

调味品中氯丙醇的GC/ECD和GC/MS/MS衍生化检测方法研究及应用

报道了调味品中氯丙醇的衍生化气相色谱(GC／ECD)和衍生化气相色谱双串联质谱法(GC／MS／MS)测定。GC／ECD测定酱油中3—氯—1，2—丙二醇(3—MCPD)的检出限达到0．01mg／kg，回收率为91％～104％，变异系数为2．27％～7．96％；GC／MS／MS同时测定酱油中1，3—二氯—2—丙醇、2，3—二氯—1—丙醇和3—氯—1，2—丙二醇，1，3—二氯—2—丙醇、2，3—二氯—1—丙醇的检出限为0．02mg／kg，3—氯—1，2—丙二醇的检出限为0．01mg／kg，回收率在92％～106％，变异系数为3．51％～13．33％。     

Quantitative evaluation of benzene, toluene, and xylene in the larvae of Drosophila melanogaster by solid-phase microextraction/gas chromatography/mass spectrometry for potential use in toxicological studies

A simple, rapid, and solvent-free method for quantitative determination of benzene, toluene, and Xylene in exposed Drosophila larvae was developed using headspace solid-phase microextraction (HS-SPME) coupled to GC/MS. Larvae fed on standard Drosophila food mixed with benzene, toluene, and Xylene for 48 h were homogenized in Milli-Q water. Extraction of benzene, toluene, and Xylene was performed at 65 degrees C for 30 min on the SPME fiber (silica-fused). Subsequently, the fiber was desorbed in the GC injection port, followed by GC/MS analysis in the selected-ion monitoring mode. An external calibration curve was used for the quantification of benzene, toluene, and Xylene in the exposed organism. Recoveries were in the range of 78-82% (intraday) and 76-81% (interday) in larvae, and 91-96% (intraday) and 87-92% (interday) in the diet. LOD with an S/N of 3:1 and LOQ with an S/N of 10:1 were in the range of 0.01-0.023 and 0.034-0.077 microg/L, respectively. Percent RSD values for benzene, toluene, and Xylene were in the range of 0.50-0.81 (intraday) and 0.89-1.23 (interday) for retention time, and 2.16--3.85 (intraday) and 2.99-4.95 (interday) for peak concentration, showing good repeatability. This method was sensitive enough to quantitate benzene, toluene, and Xylene in small exposed organisms like Drosophila larvae. The SPME/GC/MS method developed may have wider applications in various in vivo toxicological studies.     

Solid-phase microextraction-gas chromatographic determination of volatile monoaromatic hydrocarbons in soil

Benzene, toluene, ethylbenzene, three isomers of xylene, and cumene have been isolated and enriched from soil samples by a combination of water extraction at room and elevated temperature and headspace-solid-phase microextraction before their gas chromatographic-mass spectrometric (GC-MS) determination. The conditions used for all stages of sample preparation and chromatographic analysis were optimized. Analytes sampled on a polydimethylsiloxane-coated solid-phase microextraction fiber were thermally desorbed in the split/splitless injector of a gas chromatograph (GC) coupled with a mass spectrometer (MS). The desorption temperature was optimized. The GC separation was performed in a capillary column. Detection limits were found to be of the order of ca. 1 ng g(-1). Relative recoveries of the analytes from soils were found to be highly dependent on soil organic-matter content and on compound identity; they ranged from ca 92 to 96% for sandy soil (extraction at room temperature) and from ca 27 to 55% for peaty soil (extraction at elevated temperature). A few real-world soil samples were analyzed; the individual monoaromatic hydrocarbon content ranged from below detection limits to 6.4 ng g(-1) for benzene and 8.1 for the total of p- + m-xylene.     

毛细管气相色谱法测定腈纶布料中苯、甲苯和二甲基甲酰胺残留

 建立了同时定量测定腈纶布料及其服装中的苯、甲苯和二甲基甲酰胺残留的毛细管气相色谱分析方法。测得的回收率分别为 93 .3 % ,1 0 1 .8% ,94.9% ;变异系数为 3 .4% ,2 .0 % ,2 .8%。方法简便、快速、准确。     

Simultaneous Voltammetric Determination of Benzene,Toluene and Xylenes (BTX) in Water Using a Cathodically Pre‐treated Boron‐doped Diamond Electrode

An electrochemical method for the simultaneous determination of benzene, toluene and xylenes (BTX) in water was developed using square‐wave voltammetry (SWV). The determination of BTX was carried out using a cathodically pre‐treated boron‐doped diamond electrode (BDD) using 0.1 mol L^?1 H₂SO₄ as supporting electrolyte. In the SWV measurements using the BDD, the oxidation peak potentials of the total xylenes‐toluene and toluene‐benzene couples, present in ternary mixtures, display separations of about 100 and 200 mV, respectively. The attained detection limits for the simultaneous determination of benzene, toluene and total xylenes were 3.0×10^?7, 8.0×10^?7 and 9.1×10^?7 mol L^?1, respectively. The recovery values taken in ternary mixtures of benzene, toluene and total xylenes in aqueous solutions are 98.9 %, 99.2 % and 99.4 %, respectively.     

A modified method for the determination of methylmercury by gas chromatography

A simple modification of the West?? extraction procedure for methylmercury and its determination by gas chromatography (GC) is presented. The cysteine clean-up step has been modified, with use of cysteine-impregnated paper instead of cysteine solution. Methylmercury bromide is extracted from the sample into toluene and is selectively adsorbed on the cysteine paper. Interfering compounds are washed from the paper with toluene. The isolated methylmercury is set free with sulphuric acid containing bromide, extracted into benzene and determined by GC. The modification of the extraction procedure results in good recovery and reproducibility for various biological and environmental samples, good sensitivity with a detection limit of 0.1 ng/g, avoidance of difficulties arising from emulsion formation, cleaner chromatograms, and faster analysis. It is particularly suitable for determination of low levels of MeHg.     

气相色谱法同时测定溶剂型胶黏剂中的9种有害物质

建立了利用毛细管柱气相色谱同时测定溶剂型胶黏剂中苯、 甲苯、 对（间）二甲苯、 邻二甲苯、 二氯甲烷、1,2-二氯乙烷、1,1,2-三氯乙烷、三氯乙烯、甲苯二异氰酸酯（TDI）的方法,并对样品中有害物质的分离提取和色谱条件进行了研究.实验结果表明,方法化合物浓度在10~300 μg/mL时,线性相关系数不低于0.999 1,样品加标回收率在91.2%~104.1%之间,相对标准偏差均小于5%,检出限为0.1~3.0 μg/mL.方法不仅回收率高、重现性好,而且简便、快速.     

微波辅助萃取/气相色谱-质谱联用分析蔬菜中的有机磷农药

建立了微波辅助萃取（MAE）/气相色谱-质谱联用法（GC-MS）测定蔬菜样品中二嗪磷、水胺硫磷的分析方法，研究了不同溶剂的萃取效率。选择二氯甲烷为萃取溶剂，采用二因素三水平的正交设计实验优化了萃取溶剂体积和萃取时间。方法的线性范围分别为二嗪磷和对硫磷4ng/g-400ng/g，水胺硫磷20ng/g-400ng/g，检出限分别为二嗪磷和对硫磷4ng/g-400ng/g、水胺硫磷20ng/g-400ng/g，检出限分别为二嗪磷0.29ng/g、对硫磷1.70ng/g、水胺硫磷2.30ng/g。测定200.0ng/g和50.0ng/g加标蔬菜样品，回收率为72.2%-102.0%,RSD为1.5%-11.0%。与传统的机械振荡萃取法相比，不仅萃取效率相当，而且还具有省时省溶剂的优点。     

Determination of ligustilide in rat blood and tissues by capillary gas chromatography/mass spectrometry

A gas chromatography/mass spectrometry (GC/MS) method was developed to study the pharmacokinetics of ligustilide following oral administration to rats. The method was used for the analysis of samples taken from rats. Biological samples were prepared by liquid-liquid extraction (LLE) using an n-hexane-ether (2:1) solvent mixture for a sample clean-up step and analyzed by GC/MS with a quadrupole MS detector in selected ion monitoring mode (m/z 190). The calibration curves were linear over the concentration range 0.172-8.60 microg/mL (r > 0.99) for blood samples and a different range (r > 0.99) for different tissue samples. The limit of detection (LOD) was 1.0 ng/mL or 1.0 ng/g (three times the signal-noise ratio). Within- and between-day precision expressed as the relative standard deviation (RSD) for the method was 1.58-3.88 and 2.99-4.91%, respectively. The recovery for all samples was >80%, except for liver samples (>70%). The main pharmacokinetic parameters obtained were: T(max) = 0.65 +/- 0.07 h, C(max) = 1.5 +/- 0.2 microg/mL, AUC = 34 +/- 6 h microg/mL and K(a) = 3.5 +/- 0.6/h. The experimental results showed that ligustilide was easily absorbed, but its elimination was slow, from 3 to 12 h after oral administration. The concentrations of ligustilide in rat cerebellum, cerebrum, spleen and kidney were higher than those in other organs.     

Development of a gas chromatography/ion trap mass spectrometry based method for the quantification of polybrominated diphenyl ethers and polychlorinated biphenyls in adipose tissue

A combined gas chromatographic mass spectrometric (GC/MS/MS) method for the determination of seven polybrominated diphenyl ethers (PBDEs) and seven marker polychlorinated biphenyls (PCBs) in adipose tissue has been developed. Adipose tissue was melted and filtered through anhydrous sodium sulphate to obtain pure fat. Clean-up was performed using a glass column containing acidified silica, deactivated alumina and anhydrous sodium sulphate. Polybrominated biphenyl (PBB) 155 and Mirex were added as internal standards for PBDEs and PCBs, respectively. Injection standards, PBB 103 and PCB 143, for PBDEs and PCBs, respectively, were added before analysis with GC/MS/MS. The developed GC/MS/MS method has the advantage of being more selective than single MS methods because matrix effects are largely eliminated. Validation of this method was conducted according to Commission Decision 2002/657/EC. Decision limits for PBDEs and PCBs ranged from 0.06-0.15 ng g(-1) and from 0.35-1.22 ng g(-1), respectively. Detection capabilities were all between 0.23-0.55 ng g(-1) for PBDEs and between 0.98-2.29 ng g(-1) for PCBs. Precision, recovery, bias and selectivity were tested, with satisfactory results.     

Determination of Atenolol in Pharmaceutical Preparations by Gas Chromatography with Flame Ionization and Mass Spectrometric Detection

The present work describes the methodology and validation of gas chromatography with flame ionization (FID) and mass spectrometric (MS) detection after derivatization with N-Methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) for determination of atenolol with an internal standard (metoprolol) in pharmaceutical preparations. The linearity was established over the concentration range of 0.5–20 μg/mL for GC/FID and 12.5–500 ng/mL for GC/MS method. The intra- and inter-day relative standard deviation was less than 4.72 and 5.80%, respectively. Limit of quantification was determined as 500 ng/mL and 12.5 ng/mL for GC/FID and GC/MS, respectively. No interference was found from tablet excipients at the selected assay conditions. Developed GC/FID and GC/MS methods in this study are accurate, sensitive, and precise and can be easily applied to Tensinor tablet as pharmaceutical preparation.