For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatog...For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector.Parameters including extraction solvent,ionic strength,solution pH,and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water.When the described method was applied to four spiked water samples,the obtained average extraction recovery rate was found between 87%–107%and relative standard deviation was below 6%.At the same time,good linear relationships were observed for spiked water samples from 0.01 to 10μg/mL(R2=0.9993).In addition,the detection limit of salicylaldoxime was revealed between 0.003–0.008μg/mL,which is two orders of magnitude lower than previously reported results.Thus,the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.展开更多
A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrumen...A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and p H on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without Na Cl addition at p H=9. Good linearity(R2=0.9997) was obtained when the linear range was 10-500 μg/L. The recoveries of β-ionone in ultrapure water and tap water samples were 88%-95% and 110%-114%, respectively. The relative standard deviations(RSD) were less than 10%. The method detection limit(MDL) and rejection quality level(RQL) were achieved at1.98 μg/L and 6.53 μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.展开更多
为简化前处理过程,降低方法的检出限,进行了题示研究。采集鱼塘底泥样品,混匀、缩分、冷冻干燥、除杂、研磨、过筛后混匀,分取5.00 g,加入10.0μg·L^(-1)^(13)C_(6)-氯硝柳胺水合物标准溶液0.2 m L和含2.0%(体积分数)氨水的乙腈溶...为简化前处理过程,降低方法的检出限,进行了题示研究。采集鱼塘底泥样品,混匀、缩分、冷冻干燥、除杂、研磨、过筛后混匀,分取5.00 g,加入10.0μg·L^(-1)^(13)C_(6)-氯硝柳胺水合物标准溶液0.2 m L和含2.0%(体积分数)氨水的乙腈溶液20 m L,涡旋1 min,超声10 min,离心8 min。上清液于45℃旋蒸至近干,加入2.00 m L 70%(体积分数)乙腈溶液涡旋溶解残留物,再加入200 mg C18涡旋振荡30 s,离心5 min。收集上清液,过0.22μm有机滤膜,滤液采用高效液相色谱-串联质谱法测定。在色谱分析中,以Waters Atiantis^(TM) d C_(18)色谱柱为固定相,水-乙腈体系为流动相进行梯度洗脱;在质谱分析中,以电喷雾离子源负离子(ESI-)模式电离,选择反应监测(SRM)模式检测,内标法定量。结果显示,氯硝柳胺的质量浓度在0.20~50.00μg·L^(-1)内和其定量离子峰面积与同位素内标定量离子峰面积的比值呈线性关系,检出限(3S/N)为0.2μg·kg^(-1)。按照标准加入法进行回收试验,回收率为92.1%~113%,测定值的相对标准偏差(n=6)为1.6%~5.9%。方法用于实际样品的分析,检出的氯硝柳胺的质量分数为0.580~2.18 mg·kg^(-1)。展开更多
基金Project(201309052)supported by the National Special Fund for Scientific Research in the Public InterestProject(2013FJ2003)supported by the Science and Technology Planning Project of Hunan Province of China
文摘For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector.Parameters including extraction solvent,ionic strength,solution pH,and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water.When the described method was applied to four spiked water samples,the obtained average extraction recovery rate was found between 87%–107%and relative standard deviation was below 6%.At the same time,good linear relationships were observed for spiked water samples from 0.01 to 10μg/mL(R2=0.9993).In addition,the detection limit of salicylaldoxime was revealed between 0.003–0.008μg/mL,which is two orders of magnitude lower than previously reported results.Thus,the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.
基金Project(51178321)supported by the National Natural Science Foundation of ChinaProject(2012ZX07403-001)supported by the National Science and Technology Major Project,ChinaProject(20120072110050)supported by the Research Fund for the Doctoral Program of Higher Education of China
文摘A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and p H on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without Na Cl addition at p H=9. Good linearity(R2=0.9997) was obtained when the linear range was 10-500 μg/L. The recoveries of β-ionone in ultrapure water and tap water samples were 88%-95% and 110%-114%, respectively. The relative standard deviations(RSD) were less than 10%. The method detection limit(MDL) and rejection quality level(RQL) were achieved at1.98 μg/L and 6.53 μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.
文摘为简化前处理过程,降低方法的检出限,进行了题示研究。采集鱼塘底泥样品,混匀、缩分、冷冻干燥、除杂、研磨、过筛后混匀,分取5.00 g,加入10.0μg·L^(-1)^(13)C_(6)-氯硝柳胺水合物标准溶液0.2 m L和含2.0%(体积分数)氨水的乙腈溶液20 m L,涡旋1 min,超声10 min,离心8 min。上清液于45℃旋蒸至近干,加入2.00 m L 70%(体积分数)乙腈溶液涡旋溶解残留物,再加入200 mg C18涡旋振荡30 s,离心5 min。收集上清液,过0.22μm有机滤膜,滤液采用高效液相色谱-串联质谱法测定。在色谱分析中,以Waters Atiantis^(TM) d C_(18)色谱柱为固定相,水-乙腈体系为流动相进行梯度洗脱;在质谱分析中,以电喷雾离子源负离子(ESI-)模式电离,选择反应监测(SRM)模式检测,内标法定量。结果显示,氯硝柳胺的质量浓度在0.20~50.00μg·L^(-1)内和其定量离子峰面积与同位素内标定量离子峰面积的比值呈线性关系,检出限(3S/N)为0.2μg·kg^(-1)。按照标准加入法进行回收试验,回收率为92.1%~113%,测定值的相对标准偏差(n=6)为1.6%~5.9%。方法用于实际样品的分析,检出的氯硝柳胺的质量分数为0.580~2.18 mg·kg^(-1)。
