采用HPLC-MS/MS监控反应,合成了微囊藻毒素RR的谷胱甘肽和半胱氨酸代谢物(MC-RRGSH及MC-RR-Cys)。该产物经Accu BOND C18固相萃取小柱纯化后,纯度大于95%(HPLC检测)。结果表明,合成反应的最佳时间为60 min。在SPE洗脱过程中,采用纯水淋...采用HPLC-MS/MS监控反应,合成了微囊藻毒素RR的谷胱甘肽和半胱氨酸代谢物(MC-RRGSH及MC-RR-Cys)。该产物经Accu BOND C18固相萃取小柱纯化后,纯度大于95%(HPLC检测)。结果表明,合成反应的最佳时间为60 min。在SPE洗脱过程中,采用纯水淋洗,1%甲酸-90%甲醇洗脱时,MCRR-GSH和MC-RR-Cys的平均回收率可达86.4%±1.5%和90.2%±2.8%。运用ESI-HPLC-MS/MS对以上产物进行一级及二级质谱扫描。两种产物的一级质谱电离均以[M+2H]2+为基峰,对应的质荷比(m/z)分别为673.6和580.5。以MC-RR-GSH和MC-RR-Cys一级质谱图中丰度最高的双电荷离子为母离子进行二级质谱扫描,对应的子离子对为m/z 609.0/536.9和519.4/520.8,由上述裂解碎片推断合成的产物为MC-RR-GSH和MC-RR-Cys。以合成产物为标准品,测定出太湖鲤鱼肾脏中MC-RR-GSH,MC-RR-Cys和MC-RR的含量(干重)分别为未检出,1.587 5,0.001 5μg·kg-1。本文合成的高纯度代谢产物,可作为相关研究中非商品化的标准对照品,代谢产物的质谱裂解碎片亦可为环境中微囊藻毒素MC-RR的GSH/Cys代谢途径分析提供参考。展开更多
目的:建立水中微囊藻毒素LR和RR的液相色谱-串联质谱检测方法。方法:水样经C18固相萃取小柱富集,甲醇洗脱,浓缩后,经XTerra MS C18(2.1×150 mm,5μm)柱进行色谱分离,采用多反应监测(MRM)模式对微囊藻毒素进行检测,外标法定量。结果...目的:建立水中微囊藻毒素LR和RR的液相色谱-串联质谱检测方法。方法:水样经C18固相萃取小柱富集,甲醇洗脱,浓缩后,经XTerra MS C18(2.1×150 mm,5μm)柱进行色谱分离,采用多反应监测(MRM)模式对微囊藻毒素进行检测,外标法定量。结果:微囊藻毒素LR和RR的检出限分别为0.002μg/L和0.001μg/L,其加标回收率分别为84.6%～90.6%和86.6%～91.2%,相对标准偏差小于5.0%。结论:该方法用水量少,简便、快速、准确,适用于水中微囊藻毒素LR和RR的检测。展开更多
Microcystin-RR（MC-RR）,a form of microcystin with two arginine moieties,is a cyanobacterial toxin that has been detected across a wide geographic range.It is a great concern globally because of its potential liver to...Microcystin-RR（MC-RR）,a form of microcystin with two arginine moieties,is a cyanobacterial toxin that has been detected across a wide geographic range.It is a great concern globally because of its potential liver toxicity.Herein,the abilities of BiVO4,Ag-BiVO4,Ag2O-BiVO4 and Ag/Ag2O-BiVO4 to photocatalytically degrade MC-RR under visible-light irradiation（λ≥420 nm） were investigated and compared.The possible degradation pathways were explored through analysis of the reaction intermediates by high-performance liquid chromatography-mass spectrometry.The results showed that the presence of Ag^0 enhanced the photocatalytic efficiency of Ag/Ag2O-BiVO4 via a synergetic effect between Ag2O and Ag^0 at the p-n heterojunction.Moreover,the presence of Ag^0 also greatly promoted the adsorption of MC-RR on the photocatalyst surface.Toxicological experiments on mice showed that the toxicity of MC-RR was significantly reduced after photocatalytic degradation.展开更多
文摘目的:建立水中微囊藻毒素LR和RR的液相色谱-串联质谱检测方法。方法:水样经C18固相萃取小柱富集,甲醇洗脱,浓缩后,经XTerra MS C18(2.1×150 mm,5μm)柱进行色谱分离,采用多反应监测(MRM)模式对微囊藻毒素进行检测,外标法定量。结果:微囊藻毒素LR和RR的检出限分别为0.002μg/L和0.001μg/L,其加标回收率分别为84.6%～90.6%和86.6%～91.2%,相对标准偏差小于5.0%。结论:该方法用水量少,简便、快速、准确,适用于水中微囊藻毒素LR和RR的检测。
基金supported by the National Natural Science Foundation of China (21677086, 21407092, 21377067, 21577078)the Natural Science Foundation for Innovation Group of Hubei Province, China (2015CFA021)~~
文摘Microcystin-RR（MC-RR）,a form of microcystin with two arginine moieties,is a cyanobacterial toxin that has been detected across a wide geographic range.It is a great concern globally because of its potential liver toxicity.Herein,the abilities of BiVO4,Ag-BiVO4,Ag2O-BiVO4 and Ag/Ag2O-BiVO4 to photocatalytically degrade MC-RR under visible-light irradiation（λ≥420 nm） were investigated and compared.The possible degradation pathways were explored through analysis of the reaction intermediates by high-performance liquid chromatography-mass spectrometry.The results showed that the presence of Ag^0 enhanced the photocatalytic efficiency of Ag/Ag2O-BiVO4 via a synergetic effect between Ag2O and Ag^0 at the p-n heterojunction.Moreover,the presence of Ag^0 also greatly promoted the adsorption of MC-RR on the photocatalyst surface.Toxicological experiments on mice showed that the toxicity of MC-RR was significantly reduced after photocatalytic degradation.
