目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定大米、面粉、玉米、豆制品、糕点、食用油、肉制品和水果等常见食品中15种真菌毒素的分析方法。方法样品经乙腈-水...目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定大米、面粉、玉米、豆制品、糕点、食用油、肉制品和水果等常见食品中15种真菌毒素的分析方法。方法样品经乙腈-水-甲酸混合液(79:20:1,V:V:V)溶液提取后,离心机离心,上层清液用50%乙腈水溶液1:1稀释,添加同位素内标后采用HPLC-MS/MS进行检测。结果15种真菌毒素在各自范围内线性关系良好,相关系数为0.9974~1.0000;除串珠镰刀菌素(没有内标校正)外,所有毒素回收率和在低、高浓度2个添加水平的回收率为72.09%~136.58%,相对标准偏(relative standard deviation,RSD)为1.17%~27.41%(n=6),样品定量限为1~90μg/kg。结论该方法快速、准确、灵敏、成本低,适用于大米、面粉、玉米、豆制品、糕点、食用油、肉制品和水果等常见食品中15种真菌毒素的检测。展开更多
The short-and long-term stability of multi-component mixtures and intermediate mixtures of analytical standards of veterinary drugs,which can potentially occur in food and feed chains,was examined by an isochronous me...The short-and long-term stability of multi-component mixtures and intermediate mixtures of analytical standards of veterinary drugs,which can potentially occur in food and feed chains,was examined by an isochronous measurement approach.Short-term stability testing of calibrants included storage for 1,2,4,and 7 days at-20℃(as a baseline)4℃,and 23℃(with and without exposure to sunlight),respectively.Long-term stability testing conditions of intermediate mixes were-20℃,4℃,23℃(with and without exposure to sunlight),and control temperature at-80℃while the testing period was 2,4,8,and 12 weeks,respectively.Results indicated that calibration standards should ideally be stored at 4℃for only 1~2 days,without the presence of acid.Neutral storage conditions were acceptable even at room temperature.Storage of intermediate mixtures containingß-lactams and cephalosporins for longer than 1 month under 4℃ and room temperature resulted in a loss of almost 90%.When it comes to the intermediate mixtures with penicillin V and G,acceptable storage conditions were 2 weeks at-20℃,without the presence of acid.Other classes of veterinary drugs were less critical as considers long-term stability.Overall,storage conditions at-20℃were considered optimal for long-term storage of intermediate mixes of veterinary drug standards.展开更多
文摘目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定大米、面粉、玉米、豆制品、糕点、食用油、肉制品和水果等常见食品中15种真菌毒素的分析方法。方法样品经乙腈-水-甲酸混合液(79:20:1,V:V:V)溶液提取后,离心机离心,上层清液用50%乙腈水溶液1:1稀释,添加同位素内标后采用HPLC-MS/MS进行检测。结果15种真菌毒素在各自范围内线性关系良好,相关系数为0.9974~1.0000;除串珠镰刀菌素(没有内标校正)外,所有毒素回收率和在低、高浓度2个添加水平的回收率为72.09%~136.58%,相对标准偏(relative standard deviation,RSD)为1.17%~27.41%(n=6),样品定量限为1~90μg/kg。结论该方法快速、准确、灵敏、成本低,适用于大米、面粉、玉米、豆制品、糕点、食用油、肉制品和水果等常见食品中15种真菌毒素的检测。
文摘The short-and long-term stability of multi-component mixtures and intermediate mixtures of analytical standards of veterinary drugs,which can potentially occur in food and feed chains,was examined by an isochronous measurement approach.Short-term stability testing of calibrants included storage for 1,2,4,and 7 days at-20℃(as a baseline)4℃,and 23℃(with and without exposure to sunlight),respectively.Long-term stability testing conditions of intermediate mixes were-20℃,4℃,23℃(with and without exposure to sunlight),and control temperature at-80℃while the testing period was 2,4,8,and 12 weeks,respectively.Results indicated that calibration standards should ideally be stored at 4℃for only 1~2 days,without the presence of acid.Neutral storage conditions were acceptable even at room temperature.Storage of intermediate mixtures containingß-lactams and cephalosporins for longer than 1 month under 4℃ and room temperature resulted in a loss of almost 90%.When it comes to the intermediate mixtures with penicillin V and G,acceptable storage conditions were 2 weeks at-20℃,without the presence of acid.Other classes of veterinary drugs were less critical as considers long-term stability.Overall,storage conditions at-20℃were considered optimal for long-term storage of intermediate mixes of veterinary drug standards.