A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separat...A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separation of some fat-soluble components in foods. Three columns including a trap column,concentration column and analytical column were used for trapping the fat-soluble components, on-line enrichment and reverse phase separation, respectively. Capsaicinoids were on-line extracted by a CO_2 supercritical fluid, then concentrated and separated by using the C_(18) columns, finally detected by mass spectrometry(MS). Capsaicin eluted at 10.1 min and limit of detection(LOD, S/N=3) for the standard solution is 0.55pg. The linearity was calculated with a value of coefficient of determination(R^2)≥0.998 in the range of 1.1–8.5 ng. Concentrations of capsaicin in the green, yellow, and red bell peppers were determined to be 60.33 ng/g, 31.79 ng/g, 35.38ng/g, respectively.展开更多
建立了超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)快速筛查除虫菊素类农药非法添加隐性成分尼古丁含量。样品经乙酸乙酯+环己烷(1+1)溶液提取,用凝胶色谱系统GPC净化,采用CAPCELL PAK C_(18)IF2色谱柱(2.1mm×100 mm,2μm)分离...建立了超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)快速筛查除虫菊素类农药非法添加隐性成分尼古丁含量。样品经乙酸乙酯+环己烷(1+1)溶液提取,用凝胶色谱系统GPC净化,采用CAPCELL PAK C_(18)IF2色谱柱(2.1mm×100 mm,2μm)分离,0.1%甲酸(含2 mmoL乙酸铵)水溶液和乙腈为流动相进行梯度洗脱。采用电喷雾离子源正离子(ESI+)模式和多反应检测(MRM)模式进行质谱分析。尼古丁在0.2~50 ng/mL范围内线性关系良好(r^(2)=0.99966);定量限(LOQ)为0.5μg/kg,回收率为70.8%~90.5%,相对标准偏差(RSD)为4.1%~5.1%。该方法简单、准确、快速,适用于农药中非法添加隐性成分尼古丁的定性筛查和定量分析。展开更多
基金supported by the National Natural Science Foundation of China (No. 21621003)
文摘A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separation of some fat-soluble components in foods. Three columns including a trap column,concentration column and analytical column were used for trapping the fat-soluble components, on-line enrichment and reverse phase separation, respectively. Capsaicinoids were on-line extracted by a CO_2 supercritical fluid, then concentrated and separated by using the C_(18) columns, finally detected by mass spectrometry(MS). Capsaicin eluted at 10.1 min and limit of detection(LOD, S/N=3) for the standard solution is 0.55pg. The linearity was calculated with a value of coefficient of determination(R^2)≥0.998 in the range of 1.1–8.5 ng. Concentrations of capsaicin in the green, yellow, and red bell peppers were determined to be 60.33 ng/g, 31.79 ng/g, 35.38ng/g, respectively.
基金supported by the National Nature Science Foundation of China (No 30873260)the Talents Scheme from the Science and Technology Commission of Shanghai Municipality (No 09XD1403800)+2 种基金the China Postdoctoral Science Foundation (No 20090460645)the Supporting Project for Elitists in the New Century from The Ministry of Education (No NCET-07563)the Shanghai Leading Academic Discipline Project (Nos J50305 and E3008)~~
