工业用水中总铁含量的快速测定

介绍了以菲咯嗪－醋酸钠－醋酸缓冲溶液为显色体系、用自制的铁含量比色测定仪快速测定工业用水中总铁含量的方法。总铁含量≤０５ｍｇ／Ｌ时，标准偏差≤００３ｍｇ／Ｌ；总铁含量＞０５ｍｇ／Ｌ时，相对标准偏差≤５％。单次测定时间（包括样品处理）为１０～１５ｍｉｎ。采用单色光源及微型流动比色池，由蠕动泵和电子线路实现自动进样，直接显示测定结果。     

赤霉素在钼蓝法测定砷,磷,硅中的应用——连续测定钢铁中的砷,磷,硅

将植物生长刺激素赤霉素引入光度分析作新显色剂，研究了赤霉素将砷、磷、硅杂多酸还原成相应杂多蓝的显色反应。在０８４、１２０、２１６ｍｏｌ／ＬＨＣｌ介质中，赤霉素能分别将砷、磷、硅杂多酸还原成相应的杂多蓝，其最大吸收波长分别为８３５、８２０和８１０ｎｍ，表观摩尔吸光系数分别为２６４×１０４、２５４×１０４和３５１×１０４Ｌ·ｍｏｌ－１·ｃｍ－１。线性范围分别为０～２４ｍｇ／Ｌ、０～１ｍｇ／Ｌ和０～０８ｍｇ／Ｌ。该法应用于钢铁中砷、磷、硅的连续测定，结果令人满意。     

气相色谱法测定作业场所空气中的黑索金

本文报道用毛细管气相色谱电子捕获鉴定器测定作业场所空气中黑索金（ＲＤＸ）含量的新方法在优化的实验条件下，ＲＤＸ在０４０１８．０ｍｇ／Ｌ范围内可进行定量分析，检测限为０．０８ｍｇ／Ｌ，变异系数为３．９８．２％（ｎ＝６），样品回收率在９０％以上     

阿斯美胶囊中四种组分的高效液相色谱分析

建立了反相高效液相色谱法测定阿斯美胶囊中氨茶碱、盐酸甲氧非那明、马来酸氯苯那敏及那可汀四种组分的含量。色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ８，５μｍ，２００ｃｍ×４０ｍｍＩＤ，流动相为体积分数０５％的三乙胺溶液（磷酸调节ｐＨ５５）＋乙腈＋甲醇（５５０＋３６８＋８２），检测波长为２６４ｎｍ，线性范围分别为：氨茶碱３１２５～２５０ｍｇ／Ｌ，γ＝０９９９６，盐酸甲氧非那明１５６２５～１２５０ｍｇ／Ｌ，γ＝１００００，马来酸氯苯那敏２５～２００ｍｇ／Ｌ，γ＝０９９９９，那可汀８７５～７００ｍｇ／Ｌ，γ＝０９９９９；回收率（ｎ＝３）分别为１０１２％，１００８％，９９９％，９９５％；精密度：日内平均ＲＳＤ（ｎ＝６）分别为０７％，０４％，０４％，０６％；日间平均ＲＳＤ（ｎ＝３）分别为１０％，１０％，１１％，１２％。     

高效液相色谱法测定灭尔痛片的组分含量

采用高效液相色谱法同时测定灭尔痛片中对乙酰氨基酚、异丙基安替比林、及咖啡因３种成分的含量。色谱条件为：ＯＤＳ柱，甲醇＋水（６０＋４０）为流动相，检测波长为２５４ｎｍ。方法线性范围分别为：２４～１２０ｍｇ／Ｌ（ｒ＝０９９７６）；１２～６０ｍｇ／Ｌ（ｒ＝０９９９４）；４～２０ｍｇ／Ｌ（ｒ＝０９９９４）。各组分的平均回收率（ｎ＝６）分别为：１００３％，ＲＳＤ＝０４２％；９９７％，ＲＳＤ＝０６９％；９９２％，ＲＳＤ＝０４６％。该法操作简便、快捷，结果准确。     

反相高效液相色谱法直接测定茶叶水提取物中的嘌呤碱

用反相高效液相色谱法直接测定茶叶水提取物中的咖啡因、可可碱和茶碱,方法简便快速。在２７０ｎｍ检测波长下,可可碱、茶碱和咖啡因的检测下限分别为０７,０９和１８ｍｇ／Ｌ,峰面积标准曲线在６～１０００ｍｇ／Ｌ范围内具有良好的线性关系,线性相关系数为０９９８以上。     

测定亚硝酸根的表面活性剂增敏催化动力学光度法

基于在稀硫酸介质中溴化十六烷基三甲基铵对ＮＯ２－催化溴酸钾氧化曙红褪色反应的作用，建立了测定ＮＯ－２的表面活性剂增敏催化动力学光度法。加入十六烷基三甲基溴化铵（ＣＴＭＡＢ）后体系最大吸收波长由４８０ｎｍ红移至５４０ｎｍ，ΔＡ增大约２０倍。ΔＡ与ＮＯ－２含量在００１～０２ｍｇ／Ｌ范围内存在线性关系，检出限为０００４ｍｇ／Ｌ。方法已用于水样中ＮＯ－２测定，结果满意     

固相萃取—紫外导数光谱法测定血中杀鼠迷和杀鼠灵

报道了血中杀鼠迷和杀鼠灵的固相萃取－紫外导数光谱测定方法。萃取使用ＧＤＸ３０１树脂吸附，二氯乙烷洗脱。该法操作简便快速，两种杀鼠剂以１０ｍｇ／Ｌ量加于血中，回收率分别为（８２９±２１）％及（９１０±２７）％（ｘ±ＲＳＤ）。血中两种杀鼠剂的检出限分别为１５ｍｇ／Ｌ和１２ｍｇ／Ｌ。     

水杨醛苯甲酰腙高灵敏度荧光法测定土壤和水中痕量铍的研究

详细研究了铍－水杨醛苯甲酰腙（ＳＡＢＨ）荧光反应新体系的最佳条件在ｐＨ为６２介质中，试剂与铍所形成配合物的λｅｘ为３６５ｎｍ，λｅｍ为４４８ｎｍ，建立的铍荧光分析法的线性范围为０～０２０ｍｇ／Ｌ，检出下限５３×１０－４ｍｇ／Ｌ，相对标准偏差１４％，考察了４０种共存物的干扰情况。该法成功地用于土壤、污水和饮用水中痕量铍的测定。     

硫代巴比妥酸分光光度法测定消毒液中戊二醛

在醋酸介质中，硫代巴比妥酸与戊二醛生成缩合产物，此产物在可见光区有最大吸收，籍此可测定微量戊二醛。线性范围为０．５－１０．０ｍｇ／Ｌ，检出限为０．０１９ｍｇ／Ｌ。方法灵敏度高，体系简单，操作简便，用本方法测定了消毒液中戊二醛的含量，结果满意。     

High performance liquid chromatography determination of cyanide in urine by pre-column fluorescence derivatization

A method for the determination of cyanide in human urine has been developed. The method is based on the reaction of cyanide with 2,3-naphthalenedialdehyde and taurine to give a fluorescent product for reversed-phase HPLC separation and fluorometric detection. After centrifugation followed by dilution of urine samples, the specimens could be analysed directly by this method. The recovery of cyanide added to urine at concentration levels of 50-1000 pmol/mL was 85-96%. The detection limit of cyanide was 30 pmol/mL in urine. The method was successfully applied to the analysis of urine from smokers and nonsmokers. The mean concentrations of cyanide were found to be 215 pmol/mL for the former and 84 pmol/mL for the latter.     

Determination of Gentian Violet in human urine and poultry feed by high performance liquid chromatography with electrochemical detection using a carbon fibre microelectrode flow cell

A sensitive and relatively selective high performance liquid chromatographic method for the determination of Gentian Violet (GV) in human urine and chicken feed is described. The method is based on solid-phase extraction, with subsequent reversed-phase chromatographic separation on a cyano column and amperometric detection using a carbon fibre microelectrode flow cell operated at + 1.3 V. The peak currents were directly proportional to GV concentration over the concentration range 1-30 ppb (for urine samples analysis) and 1-20 ppm for poultry feed analysis. Using this method, the minimum detectable concentration was estimated to be 0.5 ppb. The method was applied successfully to the determination of GV in human urine and in chicken feed, and it was concluded that the method could be applied to the quantitative analysis of GV in the presence of its major metabolite, leuco GV. In the proposed procedure, the occurrence of matrix effects during urine analysis was significant. The electrochemical pretreatment regime described in this paper was used to overcome these effects. Recovery studies were performed on both the human urine and chicken feed samples. The recovery of GV ranged from 92 to 96% in both matrices, with a relative standard deviation of less than 5.5%.     

Analysis of Cannabinoids and Metabolites in Dried Urine Spots (DUS)

Dried urine spots (DUS) represent a potential alternative sample storage for forensic toxicological analysis. The aim of the current study was to develop and validate a liquid chromatographic tandem mass spectrometric procedure for the detection and quantitative determination of cannabinoids and metabolites in DUS. A two-step extraction was performed on DUS and urine samples. An LC-MS/MS system was operated in multiple reaction monitoring and positive polarization mode. The method was checked for sensitivity, specificity, linearity, accuracy, precision, recovery, matrix effects and carryover. The method was applied to 70 urine samples collected from healthy volunteers and drug addicts undergoing withdrawal treatment. The method was successfully developed for DUS. LODs lower than 2.0 ng/mL were obtained for all the monitored substances. All the validation parameters fulfilled the acceptance criteria either for DUS or urine. Among the real samples, 45 cases provided positive results for at least one compound. A good quali-quantitative agreement was obtained between DUS and urine. A good stability of THC, THCCOOH and THCCOOH-gluc was observed after a 24 h storage, in contrast to previously published results. DUS seems to provide a good alternative storage condition for urine that should be checked for the presence of cannabinoids and metabolites.     

A Micro-Scale Model to Monitor the Major Proteins in Human Urine Before and After Medication with Angiotensin-Converting Enzyme Inhibitor: A Preliminary Study

A simple and micro-scale liquid chromatographic (LC) method coupled with mass spectrometry was developed for analyzing major proteins in human urine. After one-step sample preparation, proteins were precipitated, redissolved, and digested. Only micro-liter level (10 μL) of urine was sufficient for major protein identification. This method was applied in clinical study, and urine proteins were monitored after medication with angiotensin-converting enzyme inhibitor within 24 hr. This method can identify many important proteins in human urine. Bioactive peptides associated with blood pressure control can also be identified simultaneously. We hope this simple method may prove useful in clinical research and disease diagnosis.     

Quantitation of sunitinib,an oral multitarget tyrosine kinase inhibitor,and its metabolite in urine samples by nonaqueous capillary electrophoresis time of flight mass spectrometry

A rapid, sensitive, and specific method was developed and validated using a nonaqueous‐capillary electrophoresis method with TOF‐MS for determination of sunitinib and N‐desethyl sunitinib in human urine. In order to avoid ionic suppression a urine samples dilution with methanol 1:10 previous step was used. This was the only treatment step to urine samples before the injection. Despite this dilution of the urine, the detection limit was as low as 0.07 mg/L for sunitinib and 0.15 mg/L for N‐desethyl sunitinib. Separation of compounds was achieved with a mixture of 5 mM ammonium formate in methanol. The calibration curves were linear over the range of 0.5–50.0 mg/L for the two analyzed compounds. The within‐run and between‐run precisions were within 5%, while the accuracy ranged from 96.0 to 100.4%. This method can be used in routine clinical practice to monitor sunitinib and N‐desethyl sunitinib drugs in the urine of cancer patients treated with once daily administration.     

Analyses of quaternary ammonium drugs in horse urine by capillary electrophoresis-mass spectrometry

A capillary electrophoresis-mass spectrometry (CE-MS) method for the analysis of quaternary ammonium drugs in equine urine was developed. Quaternary ammonium drugs were first extracted from equine urine by ion-pair extraction and then analysed by CE-MS in the positive electrospray ionization (ESI) mode. Within 12 min, eight quaternary ammonium drugs, each at 1 ng/mL in horse urine, could be detected. The confirmation of these drugs in urine samples was achieved by capillary electrophoresis tandem mass spectrometry (CE-MS/MS). A direct comparison of this method was made with existing liquid chromatography/mass spectrometry (LC-MS) methods in the detection and confirmation of glycopyrrolate and ipratropium bromide in horse urine. While the two drugs could be detected within the same CE-MS run at 1 ng/mL in urine, they could only be detected in separate LC-MS runs at 5 ng/mL in urine. In addition, CE-MS consumed a much smaller volume of extract; the analyte peak widths, in some cases, were much narrower; and as the quaternary ammonium ions were well separated electrophoretically from the mainly neutral urine matrix, a much cleaner background in the CE-MS total ion trace was observed.     

尿中有机酸的毛细管气相色谱—质谱轮廓分析—用于苯丙酮尿症的诊断

应用毛细管气相色谱-质谱轮廓分析方法,测定了33例2.5～4.5岁健康儿童尿中有机酸种类及含量和8例拟诊为苯丙酮尿症儿童尿中的有机酸,结果表明患儿尿样中苯丙酮酸、苯乙酸、邻羟基苯乙酸、对羟基苯乙酸高于正常值10～470倍。为苯丙酮尿症的确诊提供了可靠方法。     

Simultaneous determination of the flavonoid aglycones diosmetin and hesperetin in human plasma and urine by a validated GC/MS method: in vivo metabolic reduction of diosmetin to hesperetin

Diosmetin and hesperetin are the aglycones of the flavonoid glycosides diosmin and hesperidin which occur naturally in citrus fruit. A GC/MS method for the simultaneous determination of diosmetin and hesperetin in human plasma and urine has been developed and validated. The method was linear in the 2-300 ng/mL concentration range for both diosmetin and hesperetin in plasma and urine (r > 0.999). The precision of the method was better than 6.01 and 7.16% for diosmetin and hesperetin, respectively, and the accuracy was 96.76-100.40% and 95.00-105.50% for diosmetin and hesperetin, respectively. The lower limit of quantitation was found to be 2 ng/mL for both analytes in plasma and urine. Recovery of diosmetin, hesperetin and internal standard naringenin was greater than 82.5%. The method has been applied for the determination of diosmetin and hesperetin in plasma and urine samples obtained from a healthy male subject following a single oral 1000 mg dose of the flavonoid glycoside diosmin. The presence of hesperetin in plasma and urine samples indicates the metabolic reduction of diosmetin to its flavanone analogue hesperetin through reduction of the 2,3 double bond of the C-ring by the enzymes of bacteria of the intestinal microflora.     

Simultaneous quantification of six ephedrines in a Mahwang preparation and in urine by high-performance liquid chromatography

A rapid and reliable high-performance liquid chromatographic method was developed and validated for the simultaneous determination of norephedrine (NE), norpseudoephedrine (NPE), ephedrine (E), pseudoephedrine (PE), methylephedrine (ME) and methylpseudoephedrine (MPE) in both a Mahwang traditional Chinese medicine (TCM) preparation and in urine using alpha-ethylbenzylamine as the internal standard. The method uses a Spherisorb C(18) column for an isocratic elution in a tetraethylammoniumphosphate-methanol mobile phase at a wavelength of 206 nm. The limits of detection of NE, NPE, E, PE, ME and MPE in sample solutions ranged from 0.1 to 0.3 microg[sol ]mL at a signal-to-noise ratio of 3. The within-day precision as calculated from the Mahwang TCM preparation and urine samples was below 6.2 and 1.4% for each analyte. The between-day precision as calculated from the Mahwang TCM preparation and urine samples was below 6.8 and 5.9% for each analyte. The between-day accuracy as determined from the Mahwang TCM preparation and urine samples was below 2.2 and 6.8% for each analyte. The recoveries for six compounds, obtained with compounds spiked into the Mahwang TCM preparation and urine, were found to be more than 93.6%. This method can be successfully applied to doping and excretion rate studies.