该研究建立了水果中吗啉脂肪酸盐果蜡的气相色谱-三重四极杆质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)分析方法。样品使用改进QuEChERS(quick,easy,cheap,effective,rugged and safe)方法,经1%甲酸-乙腈提取,乙二胺...该研究建立了水果中吗啉脂肪酸盐果蜡的气相色谱-三重四极杆质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)分析方法。样品使用改进QuEChERS(quick,easy,cheap,effective,rugged and safe)方法,经1%甲酸-乙腈提取,乙二胺-N-丙基甲硅烷(PSA)和石墨化炭黑吸附剂(GCB)净化,使用5.5 mol/L盐酸和4.3 mol/L亚硝酸钠在冰浴条件下衍生3 h,以HP-FFAP毛细管柱进行分离,在电子轰击源(EI)和多反应监测模式下进行测定,基质曲线外标法定量。结果表明,吗啉脂肪酸盐通过亚硝基化反应可衍生成稳定的亚硝基吗啉(N-nitrosomorpholine,NMOR),目标衍生化合物峰形较好,在1~800μg/L范围内线性良好,相关系数大于0.99,检出限为0.14~1.09μg/kg,定量限为0.47~3.63μg/kg,加标回收率范围为73.6%~118.5%,相对标准偏差(RSD)为3.6%~15.2%(n=6)。该方法准确、高效,在实际样本中检出率较高,适用于水果中吗啉脂肪酸盐果蜡的定性和定量检测。展开更多
Phenolic acids (PAs) are widely found in many daily consumed vegetables and fruits.The inhibitory effects of PAs on Nnitrosomorpholine (NMOR) formation in vitro undersimulated gastric juice condition were studied. The...Phenolic acids (PAs) are widely found in many daily consumed vegetables and fruits.The inhibitory effects of PAs on Nnitrosomorpholine (NMOR) formation in vitro undersimulated gastric juice condition were studied. The results showed that the inhibjtoryIX)tency of thirteen varieties of PAs differed greatly, which may be related to theirchemical structures; the blocking rate (BR) of different killds of PAs were as follows:caf feic acid, 92.5%; tannic acid, 90.0%; gallic acid, 86.8%; sinaPinic acid, 86.2%; ferulicacid, 8l.l%; chlorogenic acid, 69.4%; gentisic acid, 69.2%; syringic acid, 62.1%; protocatechuic acid, 56.0%; p-coumaric acid, 52.5%; vannilic acid, 35.4%; moreover,p-hydroxybenzoic acid and m-coumaric acid had the least blocking effect or even slightcatalyzing effect. The results also demonstrated that amounts of NMOR formed werenegatively correlated with molar ratio of PAs to nitrite and that the optimum pH forinhibition was between 2 and 3.展开更多
文摘该研究建立了水果中吗啉脂肪酸盐果蜡的气相色谱-三重四极杆质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)分析方法。样品使用改进QuEChERS(quick,easy,cheap,effective,rugged and safe)方法,经1%甲酸-乙腈提取,乙二胺-N-丙基甲硅烷(PSA)和石墨化炭黑吸附剂(GCB)净化,使用5.5 mol/L盐酸和4.3 mol/L亚硝酸钠在冰浴条件下衍生3 h,以HP-FFAP毛细管柱进行分离,在电子轰击源(EI)和多反应监测模式下进行测定,基质曲线外标法定量。结果表明,吗啉脂肪酸盐通过亚硝基化反应可衍生成稳定的亚硝基吗啉(N-nitrosomorpholine,NMOR),目标衍生化合物峰形较好,在1~800μg/L范围内线性良好,相关系数大于0.99,检出限为0.14~1.09μg/kg,定量限为0.47~3.63μg/kg,加标回收率范围为73.6%~118.5%,相对标准偏差(RSD)为3.6%~15.2%(n=6)。该方法准确、高效,在实际样本中检出率较高,适用于水果中吗啉脂肪酸盐果蜡的定性和定量检测。
文摘Phenolic acids (PAs) are widely found in many daily consumed vegetables and fruits.The inhibitory effects of PAs on Nnitrosomorpholine (NMOR) formation in vitro undersimulated gastric juice condition were studied. The results showed that the inhibjtoryIX)tency of thirteen varieties of PAs differed greatly, which may be related to theirchemical structures; the blocking rate (BR) of different killds of PAs were as follows:caf feic acid, 92.5%; tannic acid, 90.0%; gallic acid, 86.8%; sinaPinic acid, 86.2%; ferulicacid, 8l.l%; chlorogenic acid, 69.4%; gentisic acid, 69.2%; syringic acid, 62.1%; protocatechuic acid, 56.0%; p-coumaric acid, 52.5%; vannilic acid, 35.4%; moreover,p-hydroxybenzoic acid and m-coumaric acid had the least blocking effect or even slightcatalyzing effect. The results also demonstrated that amounts of NMOR formed werenegatively correlated with molar ratio of PAs to nitrite and that the optimum pH forinhibition was between 2 and 3.
