Organophosphate nerve agents(OPNAs)are lethal chemical weapons(CWs)which hydrolyze rapidly to alkyl phosphate compounds in the environment.The identification of alkyl phosphate compounds in the environment is critical...Organophosphate nerve agents(OPNAs)are lethal chemical weapons(CWs)which hydrolyze rapidly to alkyl phosphate compounds in the environment.The identification of alkyl phosphate compounds in the environment is critical for the verification of OPNAs.Currently,due to the complex sample preparation and long detection process for organophosphate nerve agent hydrolysis products(OPNAHPs),their high-throughput determination is difficult.To simplify sample preparation and detection of OPNAHPs from environmental samples,a quick,easy,cheap,effective,rugged and safe(Qu ECh ERS)method for the simultaneous purification of the five OPNAHPs in environmental samples combined with detection through direct analysis in real-time ionization source coupled with tandem mass spectrometer(DART-MS/MS)was developed.An internal standard method was applied for the quantification.The method exhibited a good linearity(R^(2)>0.991)in the range of 1.00 ng/m L-4.00μg/m L.The limits of detection and limits of quantification were 1.00-7.00 ng/m L and 10.0-20.0 ng/m L,respectively.The recoveries of OPNAHPs in environmental samples were between 65.3%and 107%,with relative standard deviations ranged from 1.6%to 19%.In addition,the sample preparation and analysis process for OPNAHPs could be completed in less than 10 min.The results demonstrated that the modified Qu ECh ERS method could quickly and efficiently remove the matrix of environmental samples.Combined with DART-MS/MS,an accurate and high-throughput detection method of OPNAHPs in environmental samples was provided.The developed method has great potential in the fields of early warning,clinical treatment and environmental decontamination.展开更多
敞开式离子化质谱(ambient ionization mass spectrometry,AIMS)技术因其具有实时、原位分析等特点,已成为质谱学领域的一个研究热点。实时直接质谱分析(direct analysis in real-time mass spectrometry,DART-MS)作为一种典型的直接质...敞开式离子化质谱(ambient ionization mass spectrometry,AIMS)技术因其具有实时、原位分析等特点,已成为质谱学领域的一个研究热点。实时直接质谱分析(direct analysis in real-time mass spectrometry,DART-MS)作为一种典型的直接质谱分析技术,可在开放环境中实现样品的快速分析,具有性能稳定、操作简单、分析快速等优点,自2005年被报道以来,便引起了广泛的关注。本文从DART电离源的工作原理以及近2年DART-MS在环境分析、食品药品安全、生物医学分析以及公共安全等领域的应用研究进行了评述,并对其发展方向进行了展望。展开更多
Direct Analysis in Real Time Mass Spectrometry(DART-MS)was applied to identify and study the distribution profile of piperidine alkaloids in different parts of Prosopis juliflora,without isolation and separation of th...Direct Analysis in Real Time Mass Spectrometry(DART-MS)was applied to identify and study the distribution profile of piperidine alkaloids in different parts of Prosopis juliflora,without isolation and separation of the compounds by standard chromatographic techniques.With the help of DART-MS,chemical fingerprint of raw plant parts were generated,which revealed the presence of piperidine alkaloids in leaf,pod and flower.A comparative study of the distribution pattern,showed variation in the presence and distribution of these alkaloids in various parts of P.juliflora.The leaves and pod displayed the largest alkaloid pattern with a total of 12 different alkaloids in each part,whereas only 4 alkaloids were present in flower.Alkaloids:julifloridine,prosopine,prosopinine and prosafrinine were ubiquitously distributed in all the alkaloid rich plant parts.Juliprosopine was pre-eminet alkaloid in leaf,whereas pod and flower displayed copious amounts of julifloridine.展开更多
建立了采用实时直接分析-串联质谱(DART-MS/MS)对火锅底料、牛肉面汤及调味料中5种非法添加的罂粟壳生物碱进行快速筛查的方法。样品经乙腈提取净化后,在离子化温度为300℃、栅极电压为150 V、进样速率为0.8 m m/s的DART离子源正离子模...建立了采用实时直接分析-串联质谱(DART-MS/MS)对火锅底料、牛肉面汤及调味料中5种非法添加的罂粟壳生物碱进行快速筛查的方法。样品经乙腈提取净化后,在离子化温度为300℃、栅极电压为150 V、进样速率为0.8 m m/s的DART离子源正离子模式条件下进样,以电喷雾离子源正离子多反应监测(MRM)模式进行检测,实现了样品经简单预处理后使用DART-MS/MS进行检测的新方法。该方法简便、快速,能满足大批量非法添加样品的快速筛查分析要求。展开更多
依次采用石油醚、环己烷、二硫化碳、丙酮、甲醇和等体积的丙酮/二硫化碳混合溶剂对白音华褐煤(BL)进行分级萃取得到萃取物(E_1-E_6),利用甲醇、甲苯和等体积的甲醇/甲苯混合溶剂对萃取残渣进行连续热溶得到热溶物(SP_1-SP_3)。利用傅...依次采用石油醚、环己烷、二硫化碳、丙酮、甲醇和等体积的丙酮/二硫化碳混合溶剂对白音华褐煤(BL)进行分级萃取得到萃取物(E_1-E_6),利用甲醇、甲苯和等体积的甲醇/甲苯混合溶剂对萃取残渣进行连续热溶得到热溶物(SP_1-SP_3)。利用傅里叶变换红外光谱(FT-IR)、气相色谱质谱(GC/MS)和实时直接分析-质谱(DART-MS)对萃取物和热溶物的组成和结构特征进行了分析。BL总的萃取物产率和热溶物产率分别为9.37%和21.84%。E_5和E_6的FT-IR谱图中有较强的羟基吸收峰,而E_1的FT-IR谱图中脂肪C-H的伸缩振动峰强度明显高于其他萃取物;三种溶剂热溶物的FT-IR谱图相似,但SP_1和SP_3的FT-IR谱图中羟基吸收峰较强。E_1和E_5中GC/MS可检测化合物分别以烷烃和芳烃为主,E_5中还含有较多的含氧化合物;三种热溶物中化合物均以烷烃和芳烃为主,SP_3中酚类、酮类和酯类等含氧化合物的含量较高。DART-MS可检测出萃取物和热溶物中GC/MS无法检测出的较强极性和难挥发化合物;热溶物中含量较高的化合物的碳数和等价双键数(Double bond equivalent,DBE)分别集中分布在10-25和2-16,并且DBE随碳数增加而增加。展开更多
以中药为代表的天然药物具有悠久的药用历史,其功效物质基础解析和质量评价对于促进中医药的传承和创新发展具有重要意义。由于中药化学组成复杂,准确分析和鉴定与临床药效密切相关的指标成分较为困难,亟需开发和运用新型分离表征手段...以中药为代表的天然药物具有悠久的药用历史,其功效物质基础解析和质量评价对于促进中医药的传承和创新发展具有重要意义。由于中药化学组成复杂,准确分析和鉴定与临床药效密切相关的指标成分较为困难,亟需开发和运用新型分离表征手段。实时直接分析质谱(direct analysis in real-time mass spectrometry,DART-MS)是近年来新兴的常压敞开式离子化质谱技术,具有分析速度快、原位、样品前处理简单等特点。自2005年被报道以来,DART-MS在生物医学、环境监测、公共安全、药物分析等领域应用广泛。该技术为解析中药复杂化学成分和质量控制提供了新方式,具有较好的应用前景。本文概述了DART-MS技术的原理、特点、影响因素及技术进展,总结其在中药分析中的应用情况,并展望其发展前景。展开更多
辣椒是常见的调味品,对辣椒及其制品的辣度进行快速监控非常必要。该文首先对辣椒素和二氢辣椒素在实时直接质谱(direct analysis in real time mass spectrometry, DART-MS)的裂解机制进行了系统研究,进一步对DART离子源的气体解吸温...辣椒是常见的调味品,对辣椒及其制品的辣度进行快速监控非常必要。该文首先对辣椒素和二氢辣椒素在实时直接质谱(direct analysis in real time mass spectrometry, DART-MS)的裂解机制进行了系统研究,进一步对DART离子源的气体解吸温度、栅网电极电压等试验条件进行了优化。结果表明,辣椒素和二氢辣椒素质量浓度在 0.50~50.0 μg/mL 范围内与峰面积呈现良好线性关系。辣椒素和二氢辣椒素的检测限均为0.1 μg/g,定量限均为0.5 μg/g,回收率范围分别为79.74%~97.74%,85.60%~98.71%,精密度分别为0.80%~8.89%,2.69%~9.54%。该方法可用于辣椒及其制品中辣度的快速评价。展开更多
基金supported by the State Key Laboratory of NBC Protection for Civilian
文摘Organophosphate nerve agents(OPNAs)are lethal chemical weapons(CWs)which hydrolyze rapidly to alkyl phosphate compounds in the environment.The identification of alkyl phosphate compounds in the environment is critical for the verification of OPNAs.Currently,due to the complex sample preparation and long detection process for organophosphate nerve agent hydrolysis products(OPNAHPs),their high-throughput determination is difficult.To simplify sample preparation and detection of OPNAHPs from environmental samples,a quick,easy,cheap,effective,rugged and safe(Qu ECh ERS)method for the simultaneous purification of the five OPNAHPs in environmental samples combined with detection through direct analysis in real-time ionization source coupled with tandem mass spectrometer(DART-MS/MS)was developed.An internal standard method was applied for the quantification.The method exhibited a good linearity(R^(2)>0.991)in the range of 1.00 ng/m L-4.00μg/m L.The limits of detection and limits of quantification were 1.00-7.00 ng/m L and 10.0-20.0 ng/m L,respectively.The recoveries of OPNAHPs in environmental samples were between 65.3%and 107%,with relative standard deviations ranged from 1.6%to 19%.In addition,the sample preparation and analysis process for OPNAHPs could be completed in less than 10 min.The results demonstrated that the modified Qu ECh ERS method could quickly and efficiently remove the matrix of environmental samples.Combined with DART-MS/MS,an accurate and high-throughput detection method of OPNAHPs in environmental samples was provided.The developed method has great potential in the fields of early warning,clinical treatment and environmental decontamination.
文摘敞开式离子化质谱(ambient ionization mass spectrometry,AIMS)技术因其具有实时、原位分析等特点,已成为质谱学领域的一个研究热点。实时直接质谱分析(direct analysis in real-time mass spectrometry,DART-MS)作为一种典型的直接质谱分析技术,可在开放环境中实现样品的快速分析,具有性能稳定、操作简单、分析快速等优点,自2005年被报道以来,便引起了广泛的关注。本文从DART电离源的工作原理以及近2年DART-MS在环境分析、食品药品安全、生物医学分析以及公共安全等领域的应用研究进行了评述,并对其发展方向进行了展望。
文摘Direct Analysis in Real Time Mass Spectrometry(DART-MS)was applied to identify and study the distribution profile of piperidine alkaloids in different parts of Prosopis juliflora,without isolation and separation of the compounds by standard chromatographic techniques.With the help of DART-MS,chemical fingerprint of raw plant parts were generated,which revealed the presence of piperidine alkaloids in leaf,pod and flower.A comparative study of the distribution pattern,showed variation in the presence and distribution of these alkaloids in various parts of P.juliflora.The leaves and pod displayed the largest alkaloid pattern with a total of 12 different alkaloids in each part,whereas only 4 alkaloids were present in flower.Alkaloids:julifloridine,prosopine,prosopinine and prosafrinine were ubiquitously distributed in all the alkaloid rich plant parts.Juliprosopine was pre-eminet alkaloid in leaf,whereas pod and flower displayed copious amounts of julifloridine.
文摘建立了采用实时直接分析-串联质谱(DART-MS/MS)对火锅底料、牛肉面汤及调味料中5种非法添加的罂粟壳生物碱进行快速筛查的方法。样品经乙腈提取净化后,在离子化温度为300℃、栅极电压为150 V、进样速率为0.8 m m/s的DART离子源正离子模式条件下进样,以电喷雾离子源正离子多反应监测(MRM)模式进行检测,实现了样品经简单预处理后使用DART-MS/MS进行检测的新方法。该方法简便、快速,能满足大批量非法添加样品的快速筛查分析要求。
文摘依次采用石油醚、环己烷、二硫化碳、丙酮、甲醇和等体积的丙酮/二硫化碳混合溶剂对白音华褐煤(BL)进行分级萃取得到萃取物(E_1-E_6),利用甲醇、甲苯和等体积的甲醇/甲苯混合溶剂对萃取残渣进行连续热溶得到热溶物(SP_1-SP_3)。利用傅里叶变换红外光谱(FT-IR)、气相色谱质谱(GC/MS)和实时直接分析-质谱(DART-MS)对萃取物和热溶物的组成和结构特征进行了分析。BL总的萃取物产率和热溶物产率分别为9.37%和21.84%。E_5和E_6的FT-IR谱图中有较强的羟基吸收峰,而E_1的FT-IR谱图中脂肪C-H的伸缩振动峰强度明显高于其他萃取物;三种溶剂热溶物的FT-IR谱图相似,但SP_1和SP_3的FT-IR谱图中羟基吸收峰较强。E_1和E_5中GC/MS可检测化合物分别以烷烃和芳烃为主,E_5中还含有较多的含氧化合物;三种热溶物中化合物均以烷烃和芳烃为主,SP_3中酚类、酮类和酯类等含氧化合物的含量较高。DART-MS可检测出萃取物和热溶物中GC/MS无法检测出的较强极性和难挥发化合物;热溶物中含量较高的化合物的碳数和等价双键数(Double bond equivalent,DBE)分别集中分布在10-25和2-16,并且DBE随碳数增加而增加。
文摘以中药为代表的天然药物具有悠久的药用历史,其功效物质基础解析和质量评价对于促进中医药的传承和创新发展具有重要意义。由于中药化学组成复杂,准确分析和鉴定与临床药效密切相关的指标成分较为困难,亟需开发和运用新型分离表征手段。实时直接分析质谱(direct analysis in real-time mass spectrometry,DART-MS)是近年来新兴的常压敞开式离子化质谱技术,具有分析速度快、原位、样品前处理简单等特点。自2005年被报道以来,DART-MS在生物医学、环境监测、公共安全、药物分析等领域应用广泛。该技术为解析中药复杂化学成分和质量控制提供了新方式,具有较好的应用前景。本文概述了DART-MS技术的原理、特点、影响因素及技术进展,总结其在中药分析中的应用情况,并展望其发展前景。
文摘辣椒是常见的调味品,对辣椒及其制品的辣度进行快速监控非常必要。该文首先对辣椒素和二氢辣椒素在实时直接质谱(direct analysis in real time mass spectrometry, DART-MS)的裂解机制进行了系统研究,进一步对DART离子源的气体解吸温度、栅网电极电压等试验条件进行了优化。结果表明,辣椒素和二氢辣椒素质量浓度在 0.50~50.0 μg/mL 范围内与峰面积呈现良好线性关系。辣椒素和二氢辣椒素的检测限均为0.1 μg/g,定量限均为0.5 μg/g,回收率范围分别为79.74%~97.74%,85.60%~98.71%,精密度分别为0.80%~8.89%,2.69%~9.54%。该方法可用于辣椒及其制品中辣度的快速评价。
