Esters of 2- and 3-monochloropropane-1,2-diol (MCPD) are significative contaminants of processed edible oils used as foods or food ingredients. The aim of this study was to develop and validate a new method by GC-MS f...Esters of 2- and 3-monochloropropane-1,2-diol (MCPD) are significative contaminants of processed edible oils used as foods or food ingredients. The aim of this study was to develop and validate a new method by GC-MS for the simultaneous quantification of 2 and 3-MCPD esters in infant milk powder and edible vegetable oils. The developed protocol included fat fraction in infant milk powder and edible vegetable oils samples was extracted and treated with sodium methylate-methanol to cleave the ester bonds of the 2- and 3-MCPD esters, moreover, standard samples of deuterium isotope-labeled 2- and 3-MCPD palmitic acid double esters and stearic acid double esters were used as the internal standards. Furthermore, this method was validated when it was applied to food products, concrete manifestation in its good accuracy (the recovery of MCPD esters ranged from 86% to 114%), high sensitivity (the LOD of 3-MCPD and 2-MCPD esters were 0.025 and 0.020 mg/kg, LOQ were 0.075, 0.060 mg/kg, respectively) and satisfactory repeatability (RSD below 6.8%) for all analytes. In the 150 commercial edible vegetable oils and infant formula milk powder samples, we obtained a preliminary profile of MCPD ester contamination.展开更多
利用高效液相色谱仪建立一种快速、简便、确度高的测定方法来检测婴幼儿羊奶粉中的香兰素含量。样品经乙醇提取后,漩涡振动,快速离心后经微孔滤膜过滤,使用Supersil AQ C_(18)柱分离,并将甲醇-水溶液作为流动相进行梯度洗脱,在278 nm的...利用高效液相色谱仪建立一种快速、简便、确度高的测定方法来检测婴幼儿羊奶粉中的香兰素含量。样品经乙醇提取后,漩涡振动,快速离心后经微孔滤膜过滤,使用Supersil AQ C_(18)柱分离,并将甲醇-水溶液作为流动相进行梯度洗脱,在278 nm的波长下进行检测,通过外标法定量。结果表明,在0.5~50.0μg·mL^(-1)呈现良好的线性关系,线性系数为0.9998,加标回收率为96.44%~104.17%,相对标准偏差为3.30%~4.63%,香兰素的检出限为0.17μg·mL^(-1)、定量限为0.51μg·mL^(-1)。展开更多
文摘Esters of 2- and 3-monochloropropane-1,2-diol (MCPD) are significative contaminants of processed edible oils used as foods or food ingredients. The aim of this study was to develop and validate a new method by GC-MS for the simultaneous quantification of 2 and 3-MCPD esters in infant milk powder and edible vegetable oils. The developed protocol included fat fraction in infant milk powder and edible vegetable oils samples was extracted and treated with sodium methylate-methanol to cleave the ester bonds of the 2- and 3-MCPD esters, moreover, standard samples of deuterium isotope-labeled 2- and 3-MCPD palmitic acid double esters and stearic acid double esters were used as the internal standards. Furthermore, this method was validated when it was applied to food products, concrete manifestation in its good accuracy (the recovery of MCPD esters ranged from 86% to 114%), high sensitivity (the LOD of 3-MCPD and 2-MCPD esters were 0.025 and 0.020 mg/kg, LOQ were 0.075, 0.060 mg/kg, respectively) and satisfactory repeatability (RSD below 6.8%) for all analytes. In the 150 commercial edible vegetable oils and infant formula milk powder samples, we obtained a preliminary profile of MCPD ester contamination.
文摘利用高效液相色谱仪建立一种快速、简便、确度高的测定方法来检测婴幼儿羊奶粉中的香兰素含量。样品经乙醇提取后,漩涡振动,快速离心后经微孔滤膜过滤,使用Supersil AQ C_(18)柱分离,并将甲醇-水溶液作为流动相进行梯度洗脱,在278 nm的波长下进行检测,通过外标法定量。结果表明,在0.5~50.0μg·mL^(-1)呈现良好的线性关系,线性系数为0.9998,加标回收率为96.44%~104.17%,相对标准偏差为3.30%~4.63%,香兰素的检出限为0.17μg·mL^(-1)、定量限为0.51μg·mL^(-1)。
