顶空固相微萃取气相色谱法测定饮水中氯酚

目的建立顶空固相微萃取(HSSPME)气相色谱法测定水中氯酚(CPs)的方法。方法采用SPME前处理技术,用毛细色谱柱分离,电子捕获检测器检测。结果2氯酚(MCP),2,4二氯酚(DCP),2,4,6三氯酚(TCP),五氯酚(PCP)的最低检出浓度分别为60.0、2.64、0.15和0.84μgL;标准曲线的相关系数分别为0.999、0.997、0.997、0.995;样品低、中、高三种浓度的加标后回收率分别为95.3%～107%、93.6%～102%、92.4%～102%、91.5%～99.1%;相对标准偏差(n=6)分别为1.0%～8.1%、1.6%～6.6%、2.9%～8.6%、2.0%～8.2%。结论该法简便、灵敏,不使用有机溶剂,是测定氯酚类化合物的理想方法。     

尿中四氢呋喃的顶空固相微萃取-气相色谱测定法

目的 建立测定尿中四氢呋喃的顶空固相微萃取-气相色谱法.方法 以顶空固相微萃取技术处理尿样,用带氢焰离子化检测器的气相色谱仪测定尿中的四氢呋喃.通过对萃取头类型、萃取时间和温度、解吸温度和时间等影响萃取效率的因素的研究,获得了优化的试验条件.结果 在优化条件下,方法 的线性较好,样品的加标回收率为93.0%～100.8%,相对标准偏差为0.96%～3.85%,检出限可以达到0.5μg/L.结论 该方法 适用于尿中四氢呋喃的测定.

Abstract：

Objective Headspace solid-phase microextraction (HS-SPME) was used pre-concentration procedure for the determination of tetrahydrofuran in urine by gas chromatography with hydrogen flame detector. Methods Several parameters controlling SPME was studied and optimised: SPME fiber, extraction time and extraction temperature, desorption time and desorption temperature. Results Under optimal conditions, the correlation coefficient was 0.9998 and good recoveries (range from 93.0%～100.8%) were achieved,the detection limit was 0.5μg/L. Conclusion The method can be applied to the determination of trace amount of tetrahydrofuran in urine.     

Comparison between dynamic headspace and headspace solid-phase microextraction for gas chromatography of BTEX in urine

The aim of this study was to compare two extraction procedures: dynamic headspace-purge and trap (PT) and headspace solid-phase microextraction (HS-SPME) for gas chromatographic determination of benzene, toluene, ethylbenzene, and isomeric xylenes (BTEX) in urine with photoionization (PID) and mass spectrometric (MS) detection, respectively. Both methods showed linearity in the range of interest [(50-2000) ng L-1], good accuracy (80% to 100%), and repeatability (RSD< or =11%). Detection limits were in the low ng L-1 level for both methods, although slightly greater sensitivity was found for the PT method. In comparison with PT, HS-SPME was simpler and required less time for analysis. Although the analytical features of both examined methods are appropriate for biomonitoring of environmental exposure to BTEX, only the HS-SPME-GC-MS method is recommended for routine analysis of BTEX in urine. The method was applied for the quantitative analysis of BTEX in urine samples collected from non-smokers (n=10) and smokers (n=10).     

Determination of acetone, methanol, and methyl ethyl ketone in urine using head-space gas chromatography (HS.GC)]

Using HS.GC, We have succeeded in simultaneous determination of Ac, MeOH and MEK in urine without any complicated pretreatment or correction by internal standard. Moreover, in order to lower the detection limits of these materials, study was made on the salting out effect using 14 kinds of salts. As pretreatment, 2.0 ml of urine, 3.0 g of sodium sulfate and small sized magnetic stirrer are put into vial, which is sealed by septum. This is then heated for 10 min in warm bath of 50 degrees C. In order to dissolve the added salts as much as possible, the specimen is stirred by the stirrer. After cooling the liquid to room temperature, the specimen is analysed by HS.GC. The results showed that sodium sulfate was excellent synthetically. 1) Using the urine of workers not exposed to organic solvents three kinds of urine having specific gravity of 1.010, 1.024 and 1.034 were prepared and mixed standard organic solvents (Ac, MeOH and MEK) were added. Recovery percentages and coefficients of variation were calculated. The results showed that recovery percentages ranged from 92.0 to 101.7% and coefficients of variation from 0.2 to 4.6%. 2) The regression equations of standard curves were satisfactory with y = 9053x - 200(r = 0.999, n = 12) for Ac, y = 801x - 400 (r = 0.999, n = 12) for MeOH, and y = 15488x - 277 (r = 0.999, n = 12) for MEK. 3) The detection limits calculated by IUPAC formula were 0.0092 mg/l for Ac, 0.11 mg/l for MeOH and 0.0063 mg/l for MEK. These results indicated that this method is superior to other methods because the pretreatment is very simple, specificity is excellent, analysis by standard curves is possible, and this method is not affected by specific gravity of the urine.     

工业污水中挥发性有机物的顶空固相微萃取-气相色谱测定法

目的建立顶空固相微萃取-气相色谱法(SPME-GC)同时测定工业污水中苯系物、氯苯类挥发性有机物的方法。方法移取10 ml水样于15 ml样品瓶中,加入2.0 g Na Cl,在40℃平衡30 min,用聚二甲基硅氧烷(PDMS,100μm)的萃取头顶空萃取30 min后,于250℃解吸3 min。用配有HP-FFAP毛细管柱(30 m×0.32 mm,0.25μm)的7890A气相色谱仪进行分离测定。结果在4.24~8 800μg/L的线性范围内,所得12种苯系物和氯苯类挥发性有机物的回归方程均呈较好的线性关系(r0.995)。该方法的检出限为0.39~5.0μg/L,回收率在71.8%~89.6%之间,日内RSD在2.0%~5.8%之间,日间RSD在2.3%~5.9%之间。结论该方法快速、简单、检出限低、准确度高、精密度好,适合于污水中12种挥发性有机物的痕量分析检测。     

固相萃取/气相色谱法测定尿中毒鼠强含量

建立固相萃取／气相色谱法测定尿中痕量毒鼠强。尿样经C18小柱净化、毛细管气相色谱柱分离后,用氮磷检测器检测。标准曲线线性范围0．1—5μg/ml。检出限(3倍噪声)1．5pg,定量限为3ng／ml。高、低两个浓度下的回收率分别为89．3％和110％、天内精密度为10．8％和6．83％、天间精密度为2．33％和7．90％。样品在4℃冰箱中至少可以保存20d。采用该方法测定毒鼠强中毒患者的尿样,能有效地去除尿中的干扰物质,具有快速、准确、简便、灵敏度高的特点。     

测定尿中三氯乙酸的自动顶空气相色谱法

目的建立尿中三氯乙酸的自动顶空气相色谱测定方法。方法尿中的三氯乙酸加热脱羧生成三氯甲烷,经自动顶空进样器进样,解吸后进气相色谱分离,FID检测,外标法定量。结果三氯乙酸在0.1～100mg/L浓度范围内线性良好(r0.999),最低检出浓度为0.02 mg/L(v=5 ml),方法准确度高,重现性好,样品加标回收率为98.6%～99.7%,相对标准偏差(RSD)为0.8%～2.6%。结论该法简便、灵敏、准确,适用于三氯乙烯接触人群尿三氯乙酸的检测。     

Determination of benzene in urine by static headspace gas chromatography

This paper describes the application of static headspace gas chromatography in determining benzene in urine. The method was analytically validated for sensitivity (DL = 42 ng/l), repeatability (RSD = 3% and 4%), and accuracy (71%), and was applied in measuring urine benzene in nonsmokers (N = 14) and smokers (N = 18). All urine samples had measurable benzene concentrations. The method proved sensitive enough to establish a significant statistical difference (P < 0.000614) in urine benzene concentrations between smokers (mean = 760; range = 181-1869 ng/l) and nonsmokers (mean = 214; range = 61-515 ng/l).     

尿中甲酸的顶空气相色谱测定方法

在合成纤维、合成树脂、塑料、板材加工、装饰装修、食品加工、医药生产等作业场所。均存在有害物甲醛的职业性接触．新装修的居室、驾驶室等也存在甲醛危害。空气中甲醛经呼吸道吸收后，在体内进行生物转化，最终以甲酸的形式从尿液中排出。尿中甲酸可以作为职业性接触甲醛的生物标志物，测定其禽量可为评价环境受甲醛污染程度和评估人体接触甲醛剂量提供参考．该文采用顶空气相色谱法对尿中甲酸进行检测，测定结果准确可靠，重现性好。灵敏度高、方法简便快速．     

顶空固相微萃取法检测尿中丙酮

目的：建立一种测定尿中丙酮的新方法。方法：尿中的丙酮用顶空固相微萃取进行富集,经气相色谱氢焰离子化检测器检测,对萃取时间、萃取温度、转速等条件进行优选。结果：在温度为30℃、转速为中速的条件下萃取20 m in,尿丙酮线性关系良好,r在0.9994以上,相对标准偏差1.02%-4.37%,回收率在90.8%-99.5%之间。结论：顶空固相微萃取技术能用于尿中丙酮的检测。     

顶空固相微萃取气相色普法测定萝卜中有机氯农药及其代谢物

有机氯农药曾经在农业上被广泛使用,尽管我国在1983年已禁止生产使用有机氯农药[1],由于有机氯农药属于最持久稳定的有机污染物之一,且在生物体内积累,因此在环境中,特别是水、土壤中仍广泛存在.一些生长于土壤中的根茎类和块茎类食品就不可避免会受到土壤中有机氯农药的污染.因食品组成复杂,测定有机氯农药需先萃取分离和浓缩,再用气相色谱法测定.     

Biological monitoring of occupational exposure to methyl ethyl ketone by means of urinalysis for methyl ethyl ketone itself

Summary Head space gas chromatography (GC) was applied to measure methyl ethyl ketone (MEK) in urine from 62 MEK-exposed male workers, whose individual intensity of exposure to MEK was monitored utilizing the carbon felt dosimeter. The urinary MEK level increased rapidly to reach a plateau in the first quarter of the daily 8-h work, while very little MEK was detected in the preshift urine. When the MEK levels in the urine at the end of the shift were compared with the afternoon MEK-TWA values, the uncorrected MEK in urine correlated best with MEK in air (r=0.774, n=62), while correction for creatinine gave a comparable result and the correlation was poorer when corrected for a specific gravity of urine or for the lapse of time after preceding passage of urine. Balance of MEK absorption via inhalation and MEK excretion into urine revealed that only 0.1% of MEK absorbed will be excreted unchanged into urine. Wider application of head space GC is discussed for the analysis of unmetabolized solvents in urine.     

顶空气相色谱法测定水中多种挥发性卤代烃

目的：建立水中多种挥发性卤代烃的测定方法。方法：采用顶空毛细管气相色谱法测定水中碘甲烷、三氯甲烷、1,2-二氯乙烷、三氯乙烯、1,1,2-三氯乙烷、四氯乙烯、1,1,2,2-四氯乙烷、四氯化碳等8种卤代烃。结果：用建立的方法对人工合成水样进行测定,平均加标回收率为82.56%-113.69%,变异系数为1.23%-7.84%。最低检测限为0.00045-48.79μg/L。对自来水的分析中有5种卤代烃检出。结论：所建立的方法简便、快速,具有较好的精密度与准确度,可用于水中挥发性卤代烃的测定。     

顶空固相微萃取-气相色谱质谱法同时检测白酒中多种挥发性有机污染物

目的 建立白酒中33种挥发性有机污染物(VOCs)同时测定的顶空固相微萃取-气相色谱质谱检测方法。方法 将白酒的酒精度稀释成12%,取7ml放入20ml的顶空瓶,以DVB/CAR/PDMS为萃取纤维在25℃条件下萃取10min后,在200℃的气相色谱进样口中解吸3min,解吸出来的VOCs随1ml/min的载气在VF-624MS毛细管柱内得到分离,并进入四级杆质谱检测。结果 在优化后的顶空固相微萃取条件下,33种VOCs得到了较好的分离,各物质线性相关系数均大于0.99,不同水平的加标回收率在81.2%~106.6%之间,相对标准偏差均小于9%。仪器检出限和定量限分别在0.001μg/L~0.101μg/L和0.004μg/L~0.336μg/L之间。检测发现,15个白酒样品中共检出5种VOCs,甲苯的检出率及平均浓度均最高(86.7%,137.45μg/L),其次为苯乙烯,其平均检出浓度为63.12μg/L。结论 该方法适用于白酒中多种VOCs的同时、灵敏、准确地测定。白酒中存在多种VOCs的污染。     

Methyl isobutyl ketone and methyl ethyl ketone in urine as biological markers of occupational exposure to these solvents at low levels

OBJECTIVE: To examine whether unmetabolized methyl isobutyl ketone in urine is a useful marker of low-level occupational exposure to this ketone solvent, as is the case for methyl ethyl ketone. METHODS: The study was conducted in the second half of a working week. In total, 27 furniture-making workers (19 men and eight women) and 11 non-exposed controls (six men and five women) volunteered to participate in the study. Time-weighted average (TWA; 8-h) concentration of vapors of several solvents in air, including methyl isobutyl ketone (MIBK-A) and methyl ethyl ketone (MEK-A) was monitored by diffusive sampling. Urine samples collected at the end of the shift were subjected to head-space gas chromatography (GC) analysis for the unmetabolized solvents (i.e., MIBK-U and MEK-U). The relationship between the concentration of the solvent vapor and the corresponding solvent level in urine was examined by simple as well as multiple regression analysis. RESULTS: The exposures to MIBK and MEK were well below the current occupational exposure limit levels, but the maximum levels of exposure to toluene and ethylbenzene were around the corresponding exposure limit. The correlation of the TWA concentration of the solvent in air with the concentration of the corresponding solvent in the end-of-shift urine sample was significant both for MIBK and for MEK, and the correlation coefficient was larger for MIBK than for MEK. The slope in the exposure-excretion regression line was almost twice as steep for MEK than for MIBK, possibly due to the difference in water solubility. Approximately 0.12% of MIBK absorbed in the lungs will be excreted into urine, whereas the yield for MEK was somewhat higher (0.19%). CONCLUSION: MIBK in urine is a good marker of exposure to MIBK, as in the case of MEK in urine for MEK exposure.     

非职业接触人群尿中甲醇顶空气相色谱测定方法

目的 改进非职业接触人群尿中甲醇的顶空气相色谱测定方法.方法 尿样加入无水硫酸钠,在85℃条件下加热30 min,顶空法进样,经DB-WAX毛细管色谱柱(30.00m×0.32 mm ×0.25 μm)分离,氢火焰离子化检测器检测.结果 方法的最低检出浓度为6.25 μmol/L,相对标准偏差为3.2％～9.2％,平均回收率为93.3％ ～ 103.0％.结论 本方法简便、准确,可将非职业接触人群尿中的甲醇与杂质分离,适用于尿中甲醇的测定.     

固相萃取-液相色谱法测定尿液中溴敌隆

目的:建立检测中毒病人尿液中的溴敌隆的方法。方法:尿液经固相萃取柱吸附、淋洗、氮吹、定容后,用液相色谱法测定溴敌隆。结果:方法线性范围0.01 mg/L～1.0 mg/L,回归方程为Y=4.313×105X+3407,相关系数r=0.9996,检出限为0.005 mg/L,精密度(RSD)1.8%～3.6%,回收率97%～103%。结论:该方法样品提取简单快速,回收率高,精密度良好,适合测定中毒病人尿液中溴敌隆。     

比色管顶空气相色谱法测定水样中三氯甲烷

目的:建立一种水溶液中微量三氯甲烷的分析方法。方法:采用比色管顶空气相色谱法测定水样中挥发性三氯甲烷。结果:水样中挥发性三氯甲烷在0.0~12.0μg/L范围内呈良好的线性关系,r=0.9996,回收率在93%~109%之间。结论:方法操作简便,适用于各种饮用水中三氯甲烷的监测。