目的建立分散微固相萃取-高效液相色谱法测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱的含量的新方法。方法以强离子交换树脂(PCX)为吸附剂,通过对DMSPE技术中PCX用量、吸附时间、洗脱溶剂氨-乙腈浓度和洗脱体积的优化,实现样...目的建立分散微固相萃取-高效液相色谱法测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱的含量的新方法。方法以强离子交换树脂(PCX)为吸附剂,通过对DMSPE技术中PCX用量、吸附时间、洗脱溶剂氨-乙腈浓度和洗脱体积的优化,实现样品中荷叶碱的最优提取纯化。结果建立了测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分散微固相萃取-高效液相色谱法,分散微固相萃取的最佳工艺条件为:PCX用量25 mg,涡旋30 s,以3.0 mL 5%的氨-乙腈溶液进行洗脱。结论建立的含量测定方法可用于荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分析测定。该方法简单精确,稳定性高;样品处理快捷简便,溶剂损耗明显减少;设备要求低,装置简便;分析速度快,分析周期短。展开更多
目的建立分散微固相萃取-同位素内标法-超高效液相色谱-串联质谱测定水果中吗啉残留量的检测方法。方法样品经含1%甲酸的乙腈提取,经分散微固相萃取净化、超高效液相色谱BEH HILIC色谱柱分离后,经串联质谱检测,同位素内标法定量。结果...目的建立分散微固相萃取-同位素内标法-超高效液相色谱-串联质谱测定水果中吗啉残留量的检测方法。方法样品经含1%甲酸的乙腈提取,经分散微固相萃取净化、超高效液相色谱BEH HILIC色谱柱分离后,经串联质谱检测,同位素内标法定量。结果吗啉在0~200μg/L浓度范围内线性关系良好,线性相关系数为0.9998。相对标准偏差(relative standard derivation,RSD)为1.2%~2.9%,加标回收率为93.0%~101.6%。结论本方法采用同位素内标法,具有灵敏度高、精密度和准确度好等优点,简便快捷,适合水果中吗啉的日常检测工作。展开更多
基于强阳离子交换填料(PCX),采用分散微固相萃取前处理技术,结合超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用技术,建立了一种快速测定葡萄酒和啤酒中多菌灵和噻菌灵的方法。通过对分散微固相萃取技术中PCX用量、洗脱溶剂中氨水...基于强阳离子交换填料(PCX),采用分散微固相萃取前处理技术,结合超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用技术,建立了一种快速测定葡萄酒和啤酒中多菌灵和噻菌灵的方法。通过对分散微固相萃取技术中PCX用量、洗脱溶剂中氨水的体积分数、乙腈的体积分数和洗脱体积的优化,实现了样品中多菌灵和噻菌灵的有效净化。经BEH C_(18)(50 mm×2.1 mm,1.7μm)色谱柱分离后,通过静电场轨道阱质谱靶向单一离子监测(targeted single ion monitoring,tSIM)结合数据依赖的二级质谱扫描(data dependent tandem mass spectrometry,ddMS^2)采集模式进行定性定量分析。待测物多菌灵和噻菌灵在一定浓度范围内均呈良好线性关系,相关系数R^2≥0.999 9。在葡萄酒和啤酒基质中,多菌灵和噻菌灵的检出限分别为0.02和0.01μg/L,定量限分别为0.06和0.03μg/L。在0.1、1.0、100μg/L 3个添加水平下,多菌灵和噻菌灵的加标回收率分别为95.6%~110.2%和87.5%~102.8%,日内精密度(RSDr)分别为1.8%~5.2%和1.3%~4.8%,日间精密度(RSD_R)分别为4.3%~8.7%和4.8%~9.4%。该方法快速、简便、灵敏,适用于葡萄酒和啤酒中多菌灵和噻菌灵的残留检测。展开更多
Residues of tetracycline antibiotics(TCs) in environments may be harmful to human.Due to their high polarities,it is extremely challenging to efficiently enrich TCs with low concentrations in natural waters for analys...Residues of tetracycline antibiotics(TCs) in environments may be harmful to human.Due to their high polarities,it is extremely challenging to efficiently enrich TCs with low concentrations in natural waters for analysis.In this work,a magnetic metal-organic framework Fe_(3)O_(4)@[Cu_(3)(btc)_(2)]was synthesized and applied as a dispersive micro-solid phase extraction adsorbent for TCs enrichment.Effects of dispersive micro-solid phase extraction conditions including extraction time,solution p H,and elution solvent on the extraction efficiencies of TCs were investigated.Results show that TCs could be enriched efficiently by Fe_(3)O_(4)@[Cu_(3)(btc)_(2)],and electrostatic interaction between TCs and Fe_(3)O_(4)@[Cu_(3)(btc)_(2)]dominated this process.Combined with liquid chromatography-tandem mass spectrometry,four TCs residues (oxytetracycline,tetracycline,chlortetracycline,and doxycycline) in natural waters were determined.The detection limits (LOD,S/N=3) of the four antibiotics were 0.01-0.02μg/L,and the limits of quantitation (LOQ,S/N=10)were 0.04-0.07μg/L.The recoveries obtained from river water and aquaculture water spiked with three TCs concentration levels ranged from 70.3%to 96.5%with relative standard deviations of 3.8%-12.8%.Results indicate that the magnetic metal-organic framework based dispersive micro-solid phase extraction is simple,rapid and high-loading for antibiotics enrichment from water,which further expand the practical application of metal-organic frameworks in sample pretreatment for environmental pollutant analysis.展开更多
文摘目的建立分散微固相萃取-高效液相色谱法测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱的含量的新方法。方法以强离子交换树脂(PCX)为吸附剂,通过对DMSPE技术中PCX用量、吸附时间、洗脱溶剂氨-乙腈浓度和洗脱体积的优化,实现样品中荷叶碱的最优提取纯化。结果建立了测定荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分散微固相萃取-高效液相色谱法,分散微固相萃取的最佳工艺条件为:PCX用量25 mg,涡旋30 s,以3.0 mL 5%的氨-乙腈溶液进行洗脱。结论建立的含量测定方法可用于荷丹片中荷叶碱、O-去甲基荷叶碱、N-去甲基荷叶碱含量的分析测定。该方法简单精确,稳定性高;样品处理快捷简便,溶剂损耗明显减少;设备要求低,装置简便;分析速度快,分析周期短。
文摘目的建立分散微固相萃取-同位素内标法-超高效液相色谱-串联质谱测定水果中吗啉残留量的检测方法。方法样品经含1%甲酸的乙腈提取,经分散微固相萃取净化、超高效液相色谱BEH HILIC色谱柱分离后,经串联质谱检测,同位素内标法定量。结果吗啉在0~200μg/L浓度范围内线性关系良好,线性相关系数为0.9998。相对标准偏差(relative standard derivation,RSD)为1.2%~2.9%,加标回收率为93.0%~101.6%。结论本方法采用同位素内标法,具有灵敏度高、精密度和准确度好等优点,简便快捷,适合水果中吗啉的日常检测工作。
文摘基于强阳离子交换填料(PCX),采用分散微固相萃取前处理技术,结合超高效液相色谱-四级杆-静电场轨道阱高分辨质谱联用技术,建立了一种快速测定葡萄酒和啤酒中多菌灵和噻菌灵的方法。通过对分散微固相萃取技术中PCX用量、洗脱溶剂中氨水的体积分数、乙腈的体积分数和洗脱体积的优化,实现了样品中多菌灵和噻菌灵的有效净化。经BEH C_(18)(50 mm×2.1 mm,1.7μm)色谱柱分离后,通过静电场轨道阱质谱靶向单一离子监测(targeted single ion monitoring,tSIM)结合数据依赖的二级质谱扫描(data dependent tandem mass spectrometry,ddMS^2)采集模式进行定性定量分析。待测物多菌灵和噻菌灵在一定浓度范围内均呈良好线性关系,相关系数R^2≥0.999 9。在葡萄酒和啤酒基质中,多菌灵和噻菌灵的检出限分别为0.02和0.01μg/L,定量限分别为0.06和0.03μg/L。在0.1、1.0、100μg/L 3个添加水平下,多菌灵和噻菌灵的加标回收率分别为95.6%~110.2%和87.5%~102.8%,日内精密度(RSDr)分别为1.8%~5.2%和1.3%~4.8%,日间精密度(RSD_R)分别为4.3%~8.7%和4.8%~9.4%。该方法快速、简便、灵敏,适用于葡萄酒和啤酒中多菌灵和噻菌灵的残留检测。
文摘目的建立火锅底料中5种罂粟壳生物碱的超高效液相色谱-高分辨质谱检测方法。方法样品经基于强阳离子交换吸附剂(PCX)的分散微固相萃取(DMSPE)提取和净化后,以0.1%甲酸水溶液-0.1%甲酸乙腈为流动相进行梯度洗脱,HSS T3色谱柱(2.1 mm×100 mm, 1.8μm)分离,高分辨质谱平行反应监测模式采集,外标法定量。结果在给定的浓度范围内,5种罂粟壳生物碱呈良好的线性关系(R^(2)>0.999);方法检出限为0.1~0.3μg/kg,定量限为0.4~1.0μg/kg。火锅底料在1、10、100μg/kg不同加标水平中的回收率在78.5%~104.2%之间,日内精密度(RSDr)在1.8%~6.8%之间,日间精密度(RSD_(R))在4.9%~13.7%之间。结论本方法采用以PCX为吸附剂的DMSPE净化技术,在保证有效净化的基础上,简单快速、成本较低,方法灵敏度高、重现性好,可应用于固体和半固体火锅底料中5种罂粟壳生物碱的定性定量检测。
基金supported by the National Natural Science Foundation of China(No.21607003).
文摘Residues of tetracycline antibiotics(TCs) in environments may be harmful to human.Due to their high polarities,it is extremely challenging to efficiently enrich TCs with low concentrations in natural waters for analysis.In this work,a magnetic metal-organic framework Fe_(3)O_(4)@[Cu_(3)(btc)_(2)]was synthesized and applied as a dispersive micro-solid phase extraction adsorbent for TCs enrichment.Effects of dispersive micro-solid phase extraction conditions including extraction time,solution p H,and elution solvent on the extraction efficiencies of TCs were investigated.Results show that TCs could be enriched efficiently by Fe_(3)O_(4)@[Cu_(3)(btc)_(2)],and electrostatic interaction between TCs and Fe_(3)O_(4)@[Cu_(3)(btc)_(2)]dominated this process.Combined with liquid chromatography-tandem mass spectrometry,four TCs residues (oxytetracycline,tetracycline,chlortetracycline,and doxycycline) in natural waters were determined.The detection limits (LOD,S/N=3) of the four antibiotics were 0.01-0.02μg/L,and the limits of quantitation (LOQ,S/N=10)were 0.04-0.07μg/L.The recoveries obtained from river water and aquaculture water spiked with three TCs concentration levels ranged from 70.3%to 96.5%with relative standard deviations of 3.8%-12.8%.Results indicate that the magnetic metal-organic framework based dispersive micro-solid phase extraction is simple,rapid and high-loading for antibiotics enrichment from water,which further expand the practical application of metal-organic frameworks in sample pretreatment for environmental pollutant analysis.