A fast and sensitive method for determination of 8 diuretics (acetazolamide, bendroflumethiazide, bumetanide, chlorthalidone, furosemide, hydrochlorothiazide, metolazone, triamterene) and masking agent (probenecid) in...A fast and sensitive method for determination of 8 diuretics (acetazolamide, bendroflumethiazide, bumetanide, chlorthalidone, furosemide, hydrochlorothiazide, metolazone, triamterene) and masking agent (probenecid) in human urine using gas-chromatography with mass spectrometric detection is described. The extraction of the substances as function of the nature of organic solvent, mixing time and pH of aqueous phase was studied. The tandem mass spectrometry was used to increase selectivity of diuretics determination due to elimination of background interferences. Fragmentation reactions were studied for each compound and their collision energies were optimized to obtain the best selectivity. The results of method’s validation demonstrate its suitability in routine analysis for confirmation purposes.展开更多
A simple and rapid dispersive liquid–liquid microextraction(DLLME)technique coupled with gas chromatography–ion trap mass spectrometry(GC–MS)was developed for the extraction and analysis of methamphetamine(MA),peth...A simple and rapid dispersive liquid–liquid microextraction(DLLME)technique coupled with gas chromatography–ion trap mass spectrometry(GC–MS)was developed for the extraction and analysis of methamphetamine(MA),pethidine(PD),ketamine(KT)and tramadol(TD)from human urine.In this study,different parameters affecting the extraction process such as the type and volume of extraction solvent,type and volume of disperser solvent,extraction time and pH value and salt effect were studied and optimized.Under optimized conditions,the enrichment factor ranged from 185 to 226 and the average recovery ranged from 80.45%to 95.55%.The linear range was 10.0–1000.0 mg/L,the limit of detection and quantitation were in the range 0.43–1.96 mg/L and 1.44–6.53 mg/L,respectively.The relative standard deviations were in the range 1.98%–3.90%(n=7).The obtained results show that DLLME combined with GC–MS is a fast and simple method for the determination of MA,PD,KT and TD in human urine.展开更多
Source separation sanitation systems have attracted more and more attention recently.However, separate urine collection and treatment could induce odor issues, especially in large scale application. In order to avoid ...Source separation sanitation systems have attracted more and more attention recently.However, separate urine collection and treatment could induce odor issues, especially in large scale application. In order to avoid such issues, it is necessary to monitor the odor related compounds that might be generated during urine storage. This study investigated the odorous compounds that emitted from source-separated human urine under different hydrolysis conditions. Batch experiments were conducted to investigate the effect of temperature, stale/fresh urine ratio and urine dilution on odor emissions. It was found that ammonia, dimethyl disulfide, allyl methyl sulfide and 4-heptanone were the main odorous compounds generated from human urine, with headspace concentrations hundreds of times higher than their respective odor thresholds. Furthermore, the high temperature accelerated urine hydrolysis and liquid–gas mass transfer, resulting a remarkable increase of odor emissions from the urine solution. The addition of stale urine enhanced urine hydrolysis and expedited odor emissions. On the contrary, diluted urine emitted less odorous compounds ascribed to reduced concentrations of odorant precursors. In addition,this study quantified the odor emissions and revealed the constraints of urine source separation in real-world applications. To address the odor issue, several control strategies are recommended for odor mitigation or elimination from an engineering perspective.展开更多
采用液相色谱-四极杆/离子阱质谱(LC-Q/Trap-MS)建立了肌肉中16种同化甾体激素类物质(ASs)残留的同时确证及测定方法。肌肉中的ASs采用乙腈超声辅助提取,正己烷脱脂,氨基固相萃取柱净化,CAPCELL PAK C18MGⅢ柱(150 mm×2.0 mm,5.0...采用液相色谱-四极杆/离子阱质谱(LC-Q/Trap-MS)建立了肌肉中16种同化甾体激素类物质(ASs)残留的同时确证及测定方法。肌肉中的ASs采用乙腈超声辅助提取,正己烷脱脂,氨基固相萃取柱净化,CAPCELL PAK C18MGⅢ柱(150 mm×2.0 mm,5.0μm)分离,0.1%(v/v)甲酸-乙腈溶液和0.1%(v/v)甲酸-5 mmol/L甲酸铵水溶液为流动相梯度洗脱;预设定多反应监测(sMRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)模式检测,在线EPI谱库确证,内标法定量。结果表明,16种ASs在线性范围内线性关系良好(r≥0.999);定量限(LOQ,S/N≥10)为0.029～0.36μg/kg;3个添加水平(0.5、2.0和20μg/kg)下的回收率为89.9%～118%;相对标准偏差(RSD)为6.3%～16.2%。该方法准确灵敏,一次性完成16种ASs的确证和测定,可有效用于肌肉组织中ASs残留的监测分析。展开更多
目的:采用气相色谱串接质谱联用技术建立人尿中包括脱氢氯甲睾酮、美雄酮、司坦唑醇等在内的44种外源性蛋白同化类激素的确证方法。方法:根据世界反兴奋剂机构(以下简称WADA)公布的2015年版技术文件Minimum criteria for chromatographi...目的:采用气相色谱串接质谱联用技术建立人尿中包括脱氢氯甲睾酮、美雄酮、司坦唑醇等在内的44种外源性蛋白同化类激素的确证方法。方法:根据世界反兴奋剂机构(以下简称WADA)公布的2015年版技术文件Minimum criteria for chromatographic-mass spectrometric confirmation of the identity of analysis for doping control purposes(简称TD2015IDCR)的要求作为判定标准,方法验证重点考察选择性和特异性、提取回收率和稳定性等方面。结果:经验证,该方法特异性、选择性良好,符合TD2015IDCR关于确证方法的要求。结论:经过验证,该方法可检测人尿中44种外源性蛋白同化类激素,方法稳定可靠,科学有效。展开更多
文摘A fast and sensitive method for determination of 8 diuretics (acetazolamide, bendroflumethiazide, bumetanide, chlorthalidone, furosemide, hydrochlorothiazide, metolazone, triamterene) and masking agent (probenecid) in human urine using gas-chromatography with mass spectrometric detection is described. The extraction of the substances as function of the nature of organic solvent, mixing time and pH of aqueous phase was studied. The tandem mass spectrometry was used to increase selectivity of diuretics determination due to elimination of background interferences. Fragmentation reactions were studied for each compound and their collision energies were optimized to obtain the best selectivity. The results of method’s validation demonstrate its suitability in routine analysis for confirmation purposes.
文摘A simple and rapid dispersive liquid–liquid microextraction(DLLME)technique coupled with gas chromatography–ion trap mass spectrometry(GC–MS)was developed for the extraction and analysis of methamphetamine(MA),pethidine(PD),ketamine(KT)and tramadol(TD)from human urine.In this study,different parameters affecting the extraction process such as the type and volume of extraction solvent,type and volume of disperser solvent,extraction time and pH value and salt effect were studied and optimized.Under optimized conditions,the enrichment factor ranged from 185 to 226 and the average recovery ranged from 80.45%to 95.55%.The linear range was 10.0–1000.0 mg/L,the limit of detection and quantitation were in the range 0.43–1.96 mg/L and 1.44–6.53 mg/L,respectively.The relative standard deviations were in the range 1.98%–3.90%(n=7).The obtained results show that DLLME combined with GC–MS is a fast and simple method for the determination of MA,PD,KT and TD in human urine.
基金supported by the National Research Foundation,Singaporeprogram number NRF-CRP5-2009-02,for the School of Civil and Environmental Engineering/Residues and Resource Reclamation Centre,Nanyang Technological University,Singapore
文摘Source separation sanitation systems have attracted more and more attention recently.However, separate urine collection and treatment could induce odor issues, especially in large scale application. In order to avoid such issues, it is necessary to monitor the odor related compounds that might be generated during urine storage. This study investigated the odorous compounds that emitted from source-separated human urine under different hydrolysis conditions. Batch experiments were conducted to investigate the effect of temperature, stale/fresh urine ratio and urine dilution on odor emissions. It was found that ammonia, dimethyl disulfide, allyl methyl sulfide and 4-heptanone were the main odorous compounds generated from human urine, with headspace concentrations hundreds of times higher than their respective odor thresholds. Furthermore, the high temperature accelerated urine hydrolysis and liquid–gas mass transfer, resulting a remarkable increase of odor emissions from the urine solution. The addition of stale urine enhanced urine hydrolysis and expedited odor emissions. On the contrary, diluted urine emitted less odorous compounds ascribed to reduced concentrations of odorant precursors. In addition,this study quantified the odor emissions and revealed the constraints of urine source separation in real-world applications. To address the odor issue, several control strategies are recommended for odor mitigation or elimination from an engineering perspective.
文摘目的:采用气相色谱串接质谱联用技术建立人尿中包括脱氢氯甲睾酮、美雄酮、司坦唑醇等在内的44种外源性蛋白同化类激素的确证方法。方法:根据世界反兴奋剂机构(以下简称WADA)公布的2015年版技术文件Minimum criteria for chromatographic-mass spectrometric confirmation of the identity of analysis for doping control purposes(简称TD2015IDCR)的要求作为判定标准,方法验证重点考察选择性和特异性、提取回收率和稳定性等方面。结果:经验证,该方法特异性、选择性良好,符合TD2015IDCR关于确证方法的要求。结论:经过验证,该方法可检测人尿中44种外源性蛋白同化类激素,方法稳定可靠,科学有效。
