尿中马尿酸值的高效液相色谱法及正常值的探讨

在酸性条件下用高效液相色谱仪分析尿中马尿酸的含量，峰形清晰，分离效果好，无干扰，回收率及重现性均好，样品可存两周，检测限为０．０１５ｍｇ／Ｌ，变异系数（ｎ＝６）在３％以下，正常人尿中加标回收率为９５．０３％。对某石化地区非接触甲苯职工抽测，其尿中马尿酸含量在０～１２５０．７５ｍｇ／Ｌ     

尿中五氯酚的毛细管气相色谱测定方法研究

本文报道了尿中五氯酚（ＰＣＰ）的毛细管气相色谱测定方法。尿样中的ＰＣＰ经醋酐衍生、正已烷同步萃取后，毛细管色谱柱分离，电子捕获检测器检测，２，４，６－三溴酚（ＴＢＰ）作内标，峰高比定量。尿样经不同处理，可分别测定尿中游离ＰＣＰ和总的ＰＣＰ。取尿样２ｍｌ，最低检出限为２．６μｇ／Ｌ，线性范围０～６０００μｇ／Ｌ，精密度（ＲＳＤ）为３．１％～９．４％，加标回收率为８６．３％～１０１．２％。方法简便、快速、灵敏、准确。     

解毒健脾中药提取物对镉中毒的预防作用

采用ＳＤ大鼠离体气管，与重金属解毒药二巯基丁二酸（ＤＭＳＡ）对照，观察了解毒健脾中药提取物０２号（中药０２号）对呼吸道平滑肌镉染毒的保护作用。结果显示：（１）镉对气管平滑肌的抑制作用在一定范围内呈浓度依赖性。当氯化镉浓度为６ｍｍｏｌ／Ｌ，９ｍｍｏｌ／Ｌ时，气管平滑肌对乙酰胆碱的最大收缩效应（Ｅｍａｘ）从９８±３（ｎ＝６）分别降至５３±２８（ｎ＝７，Ｐ〈０．０５），１９±１５（ｎ＝７，Ｐ〈０．００１     

荧光分光光度法测定尿中微量碘

尿样用ＳｅｐｈａｎｅｘＧ－１０小柱分离，收集含Ｉ－部分，然后用Ｉ－催化砷－铈氧化还原反应和标准添加直线外推荧光分光光度法测定。本法最低检出限０．０１ｍｇ／Ｌ，尿样中Ｉ－含量在０．００１～０．０３μｇ范围内，批内相对标准偏差＜４％，批间相对标准偏差＜６％，尿样加标回收率８８％～１０４％，用本法测定１０人份随意尿样，Ｉ－浓度范围为０．０７５～０．２１３ｍｇ／Ｌ     

丙烯腈尿中代谢物—腈乙基巯基尿酸的测定

建立了柱前荧光衍生—高效液相色谱法测定丙烯腈（ＡＣＮ）在人尿中的代谢物—Ｓ－２－腈乙基巯基尿酸［Ｎ－乙酰－Ｓ－２－腈乙基半胱氨酸（ＣＥＭＡ）］。尿中ＣＥＭＡ的酸性水解产物Ｓ－２－羧乙基半胱氨酸（ＣＥＣ）与邻苯二甲醛反应生成强荧光物质。该衍生物经Ｃ１８柱分离后，用荧光检测器检测。方法检测限为３μｍｏｌ／Ｌ，尿中ＣＥＭＡ浓度为５０、２００μｍｏｌ／Ｌ时批内平均相对标准偏差为２．９％，尿加标平均回收率为９４％。ＡＣＮ现场工人的尿样经高效液相色谱—质谱联机（ＨＰＬＣ—ＭＳ）分离鉴定，确证尿中巯基尿酸结构为ＣＥＭＡ。正常人尿中未检出该化合物。该方法应用于３４例ＡＣＮ现场工人尿中ＣＥＭＡ的测定，浓度范围在３～３１６７μｍｏｌ／Ｌ     

HCl—NaBH4—K3Fe（CN）6体系气态原子吸收光谱法测定饮料中铅

采用ＶＡ－９０气态原子化装置与ＷＦＸ－１Ｄ原子吸收分光光度计联用测定饮料中铅，采用ＨＣｌ－ＮａＢＨ４－Ｋ３Ｆｅ（ＣＮ）６体系，经Ｌ９（３４）正交试验选择最佳实验条件为：ＮａＢＨ４２０ｇ／Ｌ，Ｋ３Ｆｅ（ＣＮ）６１００ｇ／Ｌ，ＨＣｌ１．５ｍｌ，氩气流量为０．８Ｌ／ｍｉｎ。在０～１００μｇ／Ｌ范围内，相关系数ｒ＝０．９９９６，回收率为９４．１％～１０７．５％，Ｒ·Ｓ·Ｄ％＝３．３～５．２特征浓度和检出限分别为１．２９μｇ／Ｌ／１％和０．０４９μｇ／Ｌ。干扰试验表明，Ｓｎ、Ｈｇ、Ｃｒ、Ｃｕ、Ｍｎ在５００μｇ／Ｌ以下，Ｚｎ、Ａｓ、Ｆｅ、Ｎｉ、Ａｇ在１０００μｇ／Ｌ以下，不干扰测定     

柑桔类水果及其果汁中D－异柠檬酸的酶法测定

本文报告了异柠檬酸脱氢酶测定柑桔类水果及其果汁中Ｄ－异柠檬酸的方法。先用碱水解法或沉淀法处理样品，以Ｄ－异柠檬酸脱氢酶和ＮＡＤＰ与之反应，在３４０ｎｍ处测定反应系统中生成的ＮＡＤＰＨ的量，即相当于Ｄ－异柠檬酸的量。在０．０２６～１．０４１ｍｍｏｌ／Ｌ含量范围内，有良好的线性关系和相关系数：Ｙ＝－０．０４２＋０．０５０８Ｘ，ｒ＝０．９９１０，变异系数（ＣＶ）为０．９％～２．６％，回收率为９４．６％～９７．３％，本法准确、简单、快速、且专一性强，不受其他杂质干扰。     

柑桔类水果及其果汁中D－异柠檬酸的酶法测定

本文报告了异柠檬酸脱氢酶测定柑桔类水果及其果汁中Ｄ－异柠檬酸的方法。先用碱水解法或沉淀法处理样品，以Ｄ－异柠檬酸脱氢酶和ＮＡＤＰ与之反应，在３４０ｎｍ处测定反应系统中生成的ＮＡＤＰＨ的量，即相当于Ｄ－异柠檬酸的量。在０．０２６～１．０４１ｍｍｏｌ／Ｌ含量范围内，有良好的线性关系和相关系数：Ｙ＝－０．０４２＋０．０５０８Ｘ，ｒ＝０．９９１０，变异系数（ＣＶ）为０．９％～２．６％，回收率为９４．６％～９７．３％，本法准确、简单、快速、且专一性强，不受其他杂质干扰。     

新银盐分光光度法测定尿中微量砷

尿样采用一次加入混合酸与钼酸钠的催化消化法，使样品前处理简便，速度加快。消化样品中的砷化物用锌加硫酸还原成砷化氢气体，经硝酸银－聚乙烯醇－乙醇溶液吸收和新银盐分光光度法测定。方法测定范围为０．０１５～０．４０ｍｇ／Ｌ，相对标准偏差３．８％～４．７％，最低检测限０．０１３ｍｇ／Ｌ。尿样加标回收率为９０．０％～１０３．２％。尿砷标样测定结果相对误差为７．０％。用本法测定４６名非接触者尿砷浓度范围为０．０１４～０．１０２ｍｇ／Ｌ。     

食物中维生素C的流动注射分析法

本文介绍了测定食物样品中维生素Ｃ（ＶＣ）的一种自动分析方法一流动注射分析法。用本方法测定了一些蔬菜和水果样品中ＶＣ的含量。结果表明，ＶＣ的标准溶液的直线回归方程为：Ｙ＝一０．００４＋ｌ，５３５×ｌ０－６ｘ（ｒ＝０．９９９５）。本方法线性好，线性范围在０．０２２７～０．２２７ｍｍｏｌ／Ｌ之间，最低检出量为０．０８μｇ。以标准参考物测定的回收率在９０％～１１０％之间，变异系数＜１０％；本方法测定结果与标准荧光法进行了比较，结果一致。本方法系自动化测定方法，操作简便，适用于测定食物中的ＶＣ。     

Thioether excretion in urine of applicators exposed to 1,3-dichloropropene: a comparison with urinary mercapturic acid excretion.

The excretion of thioethers in urine of applicators occupationally exposed to the soil fumigant 1,3-dichloropropene (DCP) was determined by the thioether assay. The mercapturic acid metabolite of E-1,3-dichloropropene, N-acetyl-S-(E-3-chloropropenyl-2-)-L-cysteine (E-DCP-MA), was the reference compound in the thioether assay. The mean recovery of E-DCP-MA was 58.5% (coefficient of variation (CV) 9%, n = 4). In non-exposed men mean background of urinary thioethers was 6.05 mmol SH/mol creatinine (n = 56). In applicators exposed to soil fumigants containing DCP, urinary excretion of thioethers followed first order elimination kinetics. Urinary half lives of elimination of thioethers were 8.0 (SD 2.5) hours based on excretion rates and 9.5 (SD 3.1) hours based on creatinine excretion. The urinary half life of elimination of thioethers was almost twofold higher compared with half lives of elimination of the mercapturic acids of Z- and E-1,3-dichloropropene. The post- minus pre-shift thioether concentrations in urine and the cumulative urinary thioether excretions correlated well with exposure to DCP. In urine samples the mean thioether concentration was 1.38 higher than mean DCP mercapturic acid concentration. This suggests the presence of unidentified thioether metabolite(s) due to exposure to soil fumigants containing DCP. According to the present data, an eight hour time weighted average exposure to the Dutch occupational exposure limit of 5 mg/m(3) DCP results in a post- minus pre-shift thioether concentration of 9.6 mmol SH/mol creatinine (95% confidence interval (95%CI) 7.4-11.8 mmol SH/mon creatinine) and in a cumulative thioether excretion of 139 micromol SH (95% CI 120-157 micromol SH). It is concluded that the thioether assay can be used to assess comparatively high levels of exposure to DCP.     

Thioether excretion in urine of applicators exposed to 1,3-dichloropropene: a comparison with urinary mercapturic acid excretion

The excretion of thioethers in urine of applicators occupationally exposed to the soil fumigant 1,3-dichloropropene (DCP) was determined by the thioether assay. The mercapturic acid metabolite of E-1,3-dichloropropene, N-acetyl-S-(E-3-chloropropenyl-2-)-L-cysteine (E-DCP-MA), was the reference compound in the thioether assay. The mean recovery of E-DCP-MA was 58.5% (coefficient of variation (CV) 9%, n = 4). In non-exposed men mean background of urinary thioethers was 6.05 mmol SH/mol creatinine (n = 56). In applicators exposed to soil fumigants containing DCP, urinary excretion of thioethers followed first order elimination kinetics. Urinary half lives of elimination of thioethers were 8.0 (SD 2.5) hours based on excretion rates and 9.5 (SD 3.1) hours based on creatinine excretion. The urinary half life of elimination of thioethers was almost twofold higher compared with half lives of elimination of the mercapturic acids of Z- and E-1,3-dichloropropene. The post- minus pre-shift thioether concentrations in urine and the cumulative urinary thioether excretions correlated well with exposure to DCP. In urine samples the mean thioether concentration was 1.38 higher than mean DCP mercapturic acid concentration. This suggests the presence of unidentified thioether metabolite(s) due to exposure to soil fumigants containing DCP. According to the present data, an eight hour time weighted average exposure to the Dutch occupational exposure limit of 5 mg/m(3) DCP results in a post- minus pre-shift thioether concentration of 9.6 mmol SH/mol creatinine (95% confidence interval (95%CI) 7.4-11.8 mmol SH/mon creatinine) and in a cumulative thioether excretion of 139 micromol SH (95% CI 120-157 micromol SH). It is concluded that the thioether assay can be used to assess comparatively high levels of exposure to DCP.     

Mercapturic acids as metabolites of alkylating substances in urine samples of German inhabitants

Hydroxyalkyl mercapturic acids (HAMA) are the main urinary metabolites of several alkylating substances that possess a carcinogenic potential, like acrolein, 1,3-butadiene, ethylene oxide, propylene oxide and glycidol. These alkylating substances are used extensively in industrial processes, but they do also occur environmentally, e.g. in tobacco smoke. The aim of this study was the determination of six HAMA, as biomarkers of exposure, in human urine of smokers and non-smokers. We applied a sensitive analytical method, using hydrophilic interaction liquid chromatography with tandem mass spectrometry (HILIC-MS/MS) for the determination of 2-hydroxyethyl mercapturic acid (HEMA, biomarker for ethylene oxide), 2-hydroxypropyl mercapturic acid (2-HPMA, biomarker for propylene oxide), 3-hydroxypropyl mercapturic acid (3-HPMA, biomarker for acrolein), 2,3-dihydroxypropyl mercapturic acid (DHPMA, biomarker for glycidol) as well as 3,4-dihydroxybutyl mercapturic acid and 3-monohydroxybutenyl mercapturic acids (DHBMA and MHBMA, biomarkers for 1,3-butadiene). Background concentrations of four HAMA were detected in each urine sample we analyzed. The mercapturic acids HEMA and MHBMA were detected in 55% and 10% of the samples, respectively. In the urine of non-smokers (n = 54) we observed median levels of 206, 1.6, 12.1, 146, 159, and <5.0 μg/g creatinine for DHPMA, HEMA, 2-HPMA, 3-HPMA, DHBMA and MHBMA, respectively. Among smokers (n = 40) median levels of DHPMA, HEMA, 2-HPMA, 3-HPMA, DHBMA and MHBMA were determined to be 217, 4.9, 46.2, 884, 211 and <5.0 μg/g creatinine, respectively. The excretion rate of the biomarkers HEMA, 2-HPMA and 3-HPMA was distinctly higher in smokers than in non-smokers. Furthermore, our study revealed a comparatively high background level of DHPMA in urine of smokers and non-smokers whose origin is still unknown. The presented data may contribute to the evaluation of reference values for urinary HAMA levels in the general population.     

尿中s-羟乙基半胱氨酸的OPA自动柱前衍生高效液相色谱法测定

目的：建立尿中s-羟乙基半胱氨酸的OPA自动性前衍生高效液相色谱法测定方法。方法：尿液经Sep-Pak C18小柱富集和纯化，样液中s-羟乙基半胱氨酸在HP1050高效液相色谱仪自动进样器中使用邻苯二甲醛（OPA）自动衍生，经Lichrospher 100RP-18e色谱柱分离，用DAD检测器在338nm波长下测定吸收值。结果：s-羟乙基半胱氨酸浓度范围0.0mmol/L-0.5mmol/L的校准曲线相关系数为0．9999，方法检出限为0．002mmol/L；s-羟乙基半胱氨酸浓度0．05mmol/L,0.30mmol/L,0.50mmol/L组内相对标准偏差（RSD）分别为1．67％、1．02％和1．40％（n=6);不同日期测定组间相对标准偏差（RSD）分别为4．78％、3．82％和3．74％（n=6)。尿中加标0．10mmol/L,0.30mmol/L的回收率分别为90％、93％。结论：方法线性好，精密度和回收率高，操作简便，自动化程度高，可用于测定尿中s-羟乙基半胱氨酸。     

尿S-羧甲基半胱氨酸的邻苯二甲醛自动柱前衍生高效液相色谱测定法

目的 探讨测定尿中S－羧甲基半胱氨酸的方法。方法 尿液经Sep-Pak C18小柱富集和纯化。样液中S－羧甲基半胱氨酸在HP1050高效液相色谱仪自动进样器中使用邻苯二甲醛（OPA）自动衍生,经Lichrospher100RP-18e色谱柱分离,用二极管阵列检测器（DAD）338nm波长下测定吸收值。结果 S－羧四基半胱氨酸浓度范围0．00－0．50mmol/L的标准曲线相关系数为0．9998,方法检出限为0．002mmol/L;S－羧甲基半胱氨酸标准溶液溶液浓度为0．05、0．30、0．50mmol/L时,测定组内相对标准偏差（RSD）分别为1．42％、0＝78％和1．97％（n＝6）;组间RSD分别为2．43％、4．23％和3．89％（n＝6）。尿中加标0．10、0．30mmol/L的回收率分别为93％、102％。结论 本线性关系好,精密度和回收率高,操作简便,自动化程度高,可用于测定尿中S－羧四基半胱氨酸。     

重型颅脑损伤患者血糖变化对预后的影响

目的探讨重型颅脑损伤患者血糖水平的变化和颅脑损伤程度及预后的关系。方法对急性重度颅脑损伤患者146例进行研究,分析其GCS评分、病死率与血糖水平的关系。结果Ⅰ组(GCS评分≤6分)即时血糖水平为(12.32±3.60)mmol/L,Ⅱ组(GCS评分6～8分)为(6.82±2.45)mmol/L,两组比较差异具有统计学意义(P<0.05);Ⅰ组24h后血糖水平为(14.50±3.44)mmol/L,Ⅱ组为(6.20±2.25)mmol/L,两组比较差异具有统计学意义(P<0.05);高血糖组死亡34例,病死率为70.83%;非高血糖组死亡25例,病死率为25.51%,两组比较差异具有统计学意义(P<0.05)。结论急性颅脑损伤后血糖水平能够作为判定病人伤情及预后的一个指标,伤者越重,血糖水平越高,其预后愈差。     

重型颅脑损伤患者血糖变化对预后的影响

目的探讨重型颅脑损伤患者血糖水平的变化和颅脑损伤程度及预后的关系。方法对急性重度颅脑损伤患者146例进行研究．分析其GCS评分、病死率与血糖水平的关系。结果Ⅰ组（GCS评分≤6分）即时血糖水平为（12．32＋3．60）mmol／L,Ⅱ组（GCS评分6～8分）为（6．82±2．45）mmol／L,两组比较差异具有统计学意义（P〈0．05）;Ⅰ组24h后血糖水平为（14．50±3．44）mmol／L．Ⅱ组为（6．20±2．25）mmol／L,两组比较差异具有统计学意义（P〈0．05）;高血糖组死亡34例,病死率为70．83％;非高血糖组死亡25例．病死率为25．51％,两组比较差异具有统计学意义（P〈0．05）。结论急性颅脑损伤后血糖水平能够作为判定病人伤情及预后的一个指标,伤者越重,血糖水平越高,其预后愈差。     

Assessing exposure to atrazine and its metabolites using biomonitoring

BACKGROUND: Atrazine (ATZ) is the second most abundantly applied pesticide in the United States. When we assessed exposure to ATZ by measuring its urinary mercapturic acid metabolite, general population data indicated that < 5% of the population was exposed to ATZ-related chemicals (limit of detection < 0.8 ng/mL). OBJECTIVES: The aim of our study was to determine if we were underestimating ATZ exposure by measuring its urinary mercapturic acid metabolite and if the urinary metabole profile changed with the exposure scenario. METHODS: We conducted a small-scale study involving 24 persons classified as high- (n = 8), low(n = 5), and environmental- (n = 11) exposed to ATZ. Using online solid phase extraction high performance liquid chromatography-tandem mass spectrometry, we measured nine ATZ-related metabolites in urine that included dealkylated, hydroxylated, and mercapturic acid metabolites. RESULTS: We found that the urinary metabolite profiles varied greatly among exposure scenarios and among persons within each exposure scenario. Although diaminochlorotriazine (DACT) appeared to be the predominant urinary metabolite detected in each exposure category, the variation in proportion of total ATZ metabolites among persons was consistently large, suggesting that one metabolite alone could not be measured as a surrogate for ATZ exposure. CONCLUSIONS: We have likely been underestimating population-based exposures by measuring only one urinary ATZ metabolite. Multiple urinary metabolites must be measured to accurately classify exposure to ATZ and its environmental degradates. Regardless, DACT and desethylatrazine appear to be the most important metabolites to measure to evaluate exposures to ATZ-related chemicals.     

离子色谱法测定尿中甲酸的含量

目的 建立一种简单、准确的检测方法,用于甲醇中毒尿样中甲酸的快速定量分析。方法 取尿样稀释、过膜,采用万通881型离子色谱仪进行分析,淋洗液为0.5 mmol/L H₂SO₄溶液,待测物分离柱为Metrosep Organic Acids有机酸交换柱,检测器为电导检测器。结果 尿中甲酸的方法检出限为0.2 mg/L,在0.5~10.0 mg/L浓度范围内线性关系良好,相关系数为0.9997,样品加标回收率在98.2%~102.7%之间,相对标准偏差(relative standard deviation,RSD)在2.8%~4.7%之间。结论 该方法前处理简单,选择性好、准确度高、精密度好,适合尿液中甲酸的快速定量测定,可为甲醇中毒调查和治疗提供参考数据。