建立使用固相萃取柱净化液态乳中14种真菌毒素(黄曲霉毒素B_1、黄曲霉毒素B_2、黄曲霉毒素G_1、黄曲霉毒素G_2、黄曲霉毒素M_1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B_1、伏马毒素B_2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯...建立使用固相萃取柱净化液态乳中14种真菌毒素(黄曲霉毒素B_1、黄曲霉毒素B_2、黄曲霉毒素G_1、黄曲霉毒素G_2、黄曲霉毒素M_1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B_1、伏马毒素B_2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、青霉酸)多残留的超高效液相色谱-串联质谱检测方法。样品经含0.1%甲酸-乙腈沉淀蛋白和提取,固相萃取柱Oasis PRi ME HLB净化后,以0.1%甲酸溶液与乙腈为流动相,经ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果表明:14种真菌毒素的定量限(R_(SN)≥10)为0.5~5μg/kg,高、中、低3个添加水平时,平均回收率为67.7%~112.7%,相对标准偏差为0.43%~7.28%。该方法的检测速度快,净化效果较好,基质干扰较少,灵敏度高,结果准确、可靠,可用于液态乳中真菌毒素的检测分析。展开更多
N-nitrosodimethylamine （NDMA） and several other N-nitrosamines have been detected as disinfection by-products in drinking waters in many countries around the world. An ultra-performance liquid chromatography- tandem...N-nitrosodimethylamine （NDMA） and several other N-nitrosamines have been detected as disinfection by-products in drinking waters in many countries around the world. An ultra-performance liquid chromatography- tandem mass spectrometry method with solid phase extraction sample preparation was developed to study the occurrence of N-nitrosamines in several water treatment plants and distribution systems in China. Isotope labeled N-nitrosodi-n-propylamine-dl4 （NDPA-dl4） was selected as the internal standard for quantification. The solid phase extraction procedures including pH, enrichment process and MS/MS parameters including capillary voltage, cone gas flow, cone voltage, collision energy were optimized to give average recoveries of 26% to 112% for nine N- nitrosamine species. The instrument detection limits were estimated to range from 0.5 to 5μg.L-1 for the nine N- nitrosamine species. NDMA and several other N-nitrosa- mines were found at fairly high concentrations in several water treatment plants and distribution systems. NDMA was found in all locations, and the highest concentrations in cities B, G, T, and W were 3.0, 35.7, 21.3, and 19.7 ng. L 1, respectively. A wide range of N-nitrosamines concentrations and species were observed in different locations. Higher concentrations of N-nitrosamines were detected in distribution systems that were further away from the treatment plants, suggesting that the contact time between the residual disinfectant and natural organic matter may play an important role in the formation of these compounds.展开更多
目的采用新型通过式固相萃取技术结合超高效液相色谱-串联质谱法(UPLC-MS/MS),建立同时测定猪肉中52种同化激素(20种雄激素、8种雌激素、10种孕激素、14种糖皮质激素)的快速方法。方法样品经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解、乙腈涡...目的采用新型通过式固相萃取技术结合超高效液相色谱-串联质谱法(UPLC-MS/MS),建立同时测定猪肉中52种同化激素(20种雄激素、8种雌激素、10种孕激素、14种糖皮质激素)的快速方法。方法样品经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解、乙腈涡旋提取后,用新型通过式固相萃取小柱Oasis PRi ME HLB净化,再经BEH C18(2.1 mm×100 mm,1.7μm)色谱柱分离,电喷雾正/负离子多反应监测模式检测,同位素内标法定量。结果 52种同化激素在相应的浓度范围内线性关系良好,相关系数均>0.997。在猪肉基质中,52种同化激素的检出限为0.1μg/kg^2μg/kg,定量限为0.3μg/kg^5μg/kg,加标回收率为62.3%~119.6%,相对标准偏差为0.6%~15.8%。结论该方法操作简便、分析速度快,灵敏度高、准确可靠,适用于猪肉中52种同化激素的同时检测。展开更多
文摘建立使用固相萃取柱净化液态乳中14种真菌毒素(黄曲霉毒素B_1、黄曲霉毒素B_2、黄曲霉毒素G_1、黄曲霉毒素G_2、黄曲霉毒素M_1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B_1、伏马毒素B_2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、青霉酸)多残留的超高效液相色谱-串联质谱检测方法。样品经含0.1%甲酸-乙腈沉淀蛋白和提取,固相萃取柱Oasis PRi ME HLB净化后,以0.1%甲酸溶液与乙腈为流动相,经ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果表明:14种真菌毒素的定量限(R_(SN)≥10)为0.5~5μg/kg,高、中、低3个添加水平时,平均回收率为67.7%~112.7%,相对标准偏差为0.43%~7.28%。该方法的检测速度快,净化效果较好,基质干扰较少,灵敏度高,结果准确、可靠,可用于液态乳中真菌毒素的检测分析。
文摘N-nitrosodimethylamine （NDMA） and several other N-nitrosamines have been detected as disinfection by-products in drinking waters in many countries around the world. An ultra-performance liquid chromatography- tandem mass spectrometry method with solid phase extraction sample preparation was developed to study the occurrence of N-nitrosamines in several water treatment plants and distribution systems in China. Isotope labeled N-nitrosodi-n-propylamine-dl4 （NDPA-dl4） was selected as the internal standard for quantification. The solid phase extraction procedures including pH, enrichment process and MS/MS parameters including capillary voltage, cone gas flow, cone voltage, collision energy were optimized to give average recoveries of 26% to 112% for nine N- nitrosamine species. The instrument detection limits were estimated to range from 0.5 to 5μg.L-1 for the nine N- nitrosamine species. NDMA and several other N-nitrosa- mines were found at fairly high concentrations in several water treatment plants and distribution systems. NDMA was found in all locations, and the highest concentrations in cities B, G, T, and W were 3.0, 35.7, 21.3, and 19.7 ng. L 1, respectively. A wide range of N-nitrosamines concentrations and species were observed in different locations. Higher concentrations of N-nitrosamines were detected in distribution systems that were further away from the treatment plants, suggesting that the contact time between the residual disinfectant and natural organic matter may play an important role in the formation of these compounds.
文摘目的采用新型通过式固相萃取技术结合超高效液相色谱-串联质谱法(UPLC-MS/MS),建立同时测定猪肉中52种同化激素(20种雄激素、8种雌激素、10种孕激素、14种糖皮质激素)的快速方法。方法样品经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解、乙腈涡旋提取后,用新型通过式固相萃取小柱Oasis PRi ME HLB净化,再经BEH C18(2.1 mm×100 mm,1.7μm)色谱柱分离,电喷雾正/负离子多反应监测模式检测,同位素内标法定量。结果 52种同化激素在相应的浓度范围内线性关系良好,相关系数均>0.997。在猪肉基质中,52种同化激素的检出限为0.1μg/kg^2μg/kg,定量限为0.3μg/kg^5μg/kg,加标回收率为62.3%~119.6%,相对标准偏差为0.6%~15.8%。结论该方法操作简便、分析速度快,灵敏度高、准确可靠,适用于猪肉中52种同化激素的同时检测。
