尿液中三氯乙酸的顶空-气相色谱法测定

本文对顶空—气相色谱法分析尿液中的三氯乙酸进行了研究 ,并讨论了平衡温度和平衡时间等因素对测定的影响 ,验证了方法的可行性。本法灵敏度高 ,重现性好 ,当尿中三氯乙酸浓度为 1、10、5 0、10 0 mg/ L时 ,相对标准偏差在 1.7%～ 2 .5 %之间 ;当尿中三氯乙酸浓度为 5、10、10 0 mg/ L时 ,回收率在98.9%～ 10 7.3%之间 ;方法的最低检出浓度为 0 .0 5 mg/ L。尿样可在 4℃冰箱中贮存 10天 ,尿中一般共存的其它溶剂对测定无干扰 ;用于现场测定与实际相符。1　仪器与试剂1.1　仪器 :气相色谱仪 :HP6 890型 GC(配氢火焰离子化检测器 ,FID) …     

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。     

辽宁省一般人群尿中三氯乙酸水平研究

目的调查辽宁省一般人群尿中三氯乙酸水平,分析其人群分布特点。方法采用多阶段分层整群随机抽样的方法,于2009—2010年从辽宁省东、中、西部三个地区抽取1289名对象进行问卷调查,并采集尿液样品,用顶空进样气相色谱法(ECD检测器)对尿样进行三氯乙酸含量的检测,通过统计分析研究一般人群尿液中三氯乙酸的分布水平。结果辽宁省一般人群尿中三氯乙酸水平的几何均数为1.84(95%CI:1.73~1.95)μg/L,P50为1.96μg/L,P95为9.72μg/L;不同年龄组人群三氯乙酸水平差异有统计学意义,其中13~16岁组尿中三氯乙酸水平最高,46~60岁组最低;不同地区尿中三氯乙酸水平有所不同;辽宁地区一般人群尿中三氯乙酸水平高于全国平均水平。结论辽宁省一般人群尿液中三氯乙酸水平在不同年龄和区域特征中均存在差异,辽宁地区一般人群尿中三氯乙酸水平高于全国平均水平。     

顶空色谱法测定尿中三氯乙酸

本文提出用顶空气相色谱法测定三氯乙烯作业工人尿中三氯乙酸。尿样于顶空小瓶中90℃恒温90min 使三氯乙酸热脱羧生成氯仿,取顶空气体用气相色谱氢焰检测器测定,以正丁醇作内标定量。方法简便,不需特殊试剂。测定结果灵敏可靠,最低检出限为0.18mg/L,日间精密度均在10%以内,加标回收率在78.0～105.8%之间。用本法测定了几十例三氯乙烯作业工人的尿液,取得了满意的结果。     

顶空气相色谱-质谱联用法测定尿中三氯乙酸

目的 建立尿中三氯乙酸(TCA)的顶空气相色谱-质谱联用测定方法.方法 尿中TCA加热脱羧生成三氯甲烷,经三合一自动进样器顶空进样,气相色谱柱分离,质谱检测器检测.结果 TCA在0.061 1 ～ 305.436 8 μmol/L范围内线性良好(相关系数＞0.999),最低检出浓度为0.009 2 μmol/L(V=3 nl),不同浓度的相对标准偏差为4.5％ ～8.7％,样品加标回收率为82.0％ ～98.3％.结论 本法简便、灵敏、准确,可同时应用于正常人群、职业接触人群和中毒病人的尿TCA的检测.     

健康成人尿中三氯乙酸生物限值及其测定方法的探讨

目的探讨深圳市健康成人尿液中三氯乙酸生物限值,为深圳市乃至全国提供三氯乙烯中毒诊断的参考指标。方法筛选250名无职业性三氯乙烯接触史的健康成人,分为男女2组。采集尿液,测量比重,用FFAP色谱柱分离,氢火焰离子化检测器检测,以保留时间定性,峰面积定量。结果该方法的最低检出浓度为0.15mg/L,在0～80.0mg/L范围内线性关系良好,平均回收率为98.50%～100.67%。250名健康成人尿中三氯乙酸测定范围为5.80～225.10mg/L,平均浓度为64.72mg/L,相对标准偏差为1.80,95%上限值为169.40mg/L。男女2组经t检验,差异无统计学意义(t=0.53,P0.05)。结论建议深圳市健康成人尿液三氯乙酸生物限值上限为169.40mg/L。     

离子色谱法测定尿中三氯乙酸

目的:建立尿中三氯乙酸(TCA)的简便快速离子色谱法。方法:用AS19阴离子分析柱1,0 mmol～35 mmol KOH淋洗液,流速为1.00 ml/min,电导检测器。样品经高速离心用0.25μm微孔滤膜过滤稀释后直接进样。结果:本法相关性好(r=0.9998),精密度高(RSD<5.0),样品平均加标回收率为97.0%～101.2%,检出限为0.06 mg/L。结论:该方法操作简便、快速、灵敏、实用,适用于应急样品和大批尿样分析。     

尿中三氯乙酸测定的顶空固相微萃取气质联用法

目的 建立尿中三氯乙酸的顶空固相微萃取气质联用测定方法.方法 尿中的三氯乙酸加热脱羧生成三氯甲烷,经顶空固相微萃取提取,解吸后进气相色谱分离,质谱检测器检测.结果 三氯乙酸在1～1000μg/L浓度范围内线性良好,线性方程为y=613.1X +4801( r=0.9996),最低检出浓度为0.4 μg/L,样品加标回收率93.3％～100.7％,相对标准偏差为1.3％～6.7％.结论 该法简便、灵敏、准确,可应用于正常人群尿液中三氯乙酸的检测.     

气相色谱法测定水中氯乙酸的研究

[目的 ]建立一种简便、准确、适于基层使用的测定水中氯乙酸方法。 [方法 ]用酸、甲醇酯化氯乙酸 ,15 ?GS填充色谱柱分离 ,电子捕获检测器检测。 [结果 ]氯乙酸最佳酯化条件 :温度 60℃ ,时间 60min ,浓硫酸 0 4ml,甲醇0 8ml。色谱最佳测试条件 :15 ?GS色谱柱分离 ,柱温 10 5℃ ,气化室温度 190℃ ,检测室温度 190℃。该法线性范围较宽 ,一氯乙酸线性范围在 2 5～ 40 0 μg/ml(r=0 993 9) ,三氯乙酸线性范围在 0 2 5～ 1 0 μg/ml(r =0 9940 ) ,回收率在 95 %～ 10 5 %之间 ,CV均小于 5 % ,显示出良好的精密度和准确度。 [结论 ]本法具有快速、灵敏、准确等优点 ,是适于基层使用的一种分析方法     

静态顶空-毛细管柱气相色谱法检测水中甲基叔丁基醚

目的:建立适用于水中甲基叔丁基醚的静态顶空气相色谱测定方法。方法:采用静态顶空极性毛细管柱气相色谱法测定水中甲基叔丁基醚。结果:在所建立的实验条件下水中甲基叔丁基醚的检出限为0.0163μg/L,线性范围为0.0156~120 mg/L,其相关系数r=0.9997,样品的加标回收率为92.6%~100.1%,相对标准偏差(RSD)低于1.1%。结论:此方法能够用于分析水中甲基叔丁基醚。     

Simple microdetermination of trichloroethanol glucuronide and trichloroacetic acid in urine

Summary A microdetermination of estimating urinary trichloroethanol glucuronide and trichloroacetic acid is described. The glucuronide of trichloroethanol in urine was hydrolysed and oxidized to trichloroacetic acid by chromium trioxide. Trichloroacetic acid thus produced was allowed to react with pyridine and potassium hydroxide in a boiling water bath, and the product was treated with benzidine dihydrochloride or less toxic p-toluidine hydrochloride. In the urine containing trichloroethanol glucuronide and trichloroacetic acid, total trichloro-compound was obtained after oxidation to trichloroacetic acid. The assay of trichloroacetic acid is identical with the above except that digestion step was omitted. And the difference between the two results was considered to estimate the trichloroethanol content.The analytical sensitivity of this reaction is about 4 times as much as the pyridine potassium hydroxide reaction. Direct microdetermination for urinary trichloroacetic acid is also estimated.     

Measurement of chloral hydrate,trichloroethanol, trichloroacetic acid and monochloroacetic acid in the serum and the urine by gas chromatography

Summary A gas chromatographic method for the determination of trichloroethylene metabolites in the serum and the urine is described.The trichloroethanol glucuronide in the urine was hydrolyzed to trichloroethanol by -glucuronidase. After an extraction with ethyl ether, the extract was dried at 20C, then the residue was extracted with n-hexane and was injected into a gas Chromatograph.Trichloroacetic acid and monochloroacetic acid in the urine were extracted with ethyl ether. After evaporation of the ethyl ether, the acids were methylated with methanolic hydrogen chloride, by heating, and the residue was taken up in n-hexane and was injected into a gas chromatograph. The peak-areas on the gas chromatogram of the trichloroethylene, chloral hydrate and methyl esters of trichloroacetic acid and monochloroacetic acid were measured respectively, using a calibration curve prepared in the same conditions.Procedure for measuring trichloro-compounds in the serum was the same as for that in the urine, except that the ethyl ether extraction of trichloro-compounds was conducted after deproteinization.The serum concentration of trichloro-compounds in the rabbit, after administering trichloroethylene orally, reached the maximum in the following order: trichloroethylene and chloral hydrate > free trichloroethanol, trichloroethanol glucuronide and monochloroacetic acid > trichloroacetic acid. The urinary metabolites of trichloroethylene did so in the following order: free trichloroethanol and monochloroacetic acid > trichloroethanol glucuronide > trichloroacetic acid.Read before the 45th Annual Meeting of Japan Industrial Health Association, Tokyo, April 8, 1972.     

生活饮用水中二氯乙酸和三氯乙酸的离子色谱电导测定法

目的:建立生活饮用水中二氯乙酸(DCAA)和三氯乙酸(TCAA)的离子色谱检测法。方法:利用Dionex 2100型离子色谱仪,选用IonPac AS19阴离子色谱分析柱,进样体积500μl,10 mmol/L～45 mmol/L氢氧化钾溶液梯度淋洗,流速1.0 ml/min,电导检测器,0.22μm滤膜过滤后直接进样。结果:本法相关性r>0.999,DCAA和TCAA最低检出限分别为0.003 mg/L和0.005 mg/L,RSD%<4.56%,回收率范围85%～104%。结论:本法具有简便快速,灵敏准确及安全实用的特点,适合生活饮用水大批样品的检测。     

尿中三甲基氯化锡的顶空-气相色谱测定法

目的 建立测定尿中三甲基氯化锡的顶空-气相色谱法.方法 尿样中三甲基氯化锡经衍生后用顶空-气相色谱进行分离,定性定量检测.结果 在0.02～0.40 mg/L浓度范围内尿中三甲基氯化锡呈二次曲线,r=0.999 2,检出限为0.005 mg/L,相对标准偏差为1.9%～2.5%,回收率为92.0%～100.0%,尿样在-18 ℃冰箱中至少可以保存90d.结论 本法对于检测中所用的仪器、试剂要求较低,样品处理简便,方法 灵敏度高,干扰少,重现性好,适用于定性和定量分析,便于推广.

Abstract：

Objective To establish a detection method for trimethyltin chloride in urine by the Head space-GC. Method After derivatizing trimethyltin chloride, the urines was separated by the head space-gc,and then the trimethyltin chloride detected qualitatively and quantificationally. Results In the concentration range of 0.02～0.40 mg/L urinary trimethyltin chloride, showed a quadratic, r = 0.999 2,detection limit was 0.005 mg/L, the relative standard deviation was 1.9%～2.5%, recovery was 92.0% to 100%,the urine samples can be saved at least 90 days in -18 ℃ refrigerator. Conclusion The instrument,reagents involved in the detection require low, the operations to processing samples are simple, high sensitivity, less interference, good reproducibility, and suitable for quantitative and qualitative analysis,convenient to promotion.