三聚氰胺的毒性研究
毒理学杂志2008 年6 月第22 卷第3 期
J Toxicol June 2008 Vol122 No13
喂三聚氰胺后肾脏肾小管中出现了晶体。由此推断三
聚氰胺长期饲喂可能引起肾衰竭。
国内已经有采用高效液相色谱法(HPLC) 法
检测饲料和工业品的三聚氰胺的含量 ,该方法更为
灵敏,简单。
吴明礼,陈彩虹. 高效液相色谱法(HPLC) 测定单氰胺中
三聚氰胺的含量. 宁夏石油化工,2005 ,2 :24225.
辜雪英,吴小花,仇满珍. 饲料中三聚氰胺残留量高效液
相色谱测定的研究. 江西化工,2007 ,2 :18222.
帮发附件
饲料中三聚氰胺残留量高效液相色谱测定的研究.pdf (133.19k)
看看过WU君提供的资料，谢过，又明白了一点。
老美的猫阿狗阿出事的时候？用什么方法检出鉴定的Melamine？
What up？What new？
现在是用什么方法认定“重大食品安全事件”的呢？
FDA最新方法（2007-4-2）
Updated FCC Developmental Melamine Quantitation (HPLC-UV)
April 2, 2007
Sample Preparation/Extraction:
Wheat gluten: Ground in a Retsch ZM 100 centrifugal rotor mill (ring sieve 0.5 mm).
Moist pet food: Moist chunks and gravy were blended to the consistency of a gritty pudding prior to sampling.
Samples weighed into glass scintillation vials. Extract using 50:50 acetonitrile:water.
Procedure: Add indicated volume of extraction solvent (see note below) 1. Cap and vortex thoroughly, get aggressive with this step (critical due to slow dissolution rate of melamine). Sonicate 30 minutes. Filter portion of extract through 2-stage GMF-nylon (0.45 m m) filters. Dilute filtered extract 250 ml extract + 750 ml solvent 2 to maintain solubility of matrix components.
1 Wheat gluten: Extract in proportion 0.1 g to 10 ml. For melamine contents above 2% w/w, extract in proportion 0.05 g to 15 ml.
1 Moist pet food: Extract in proportion 2.0 – 2.5 g to 10 ml.
2 Solvent for final dilution may be water or 0.1 N HCl. Final dilution is necessary for compatibility with ion-pairing chromatography. We have observed some differences in behavior between the wheat gluten and pet food samples with respect to maintaining solubility during final dilution (these are most likely matrix components which fall out). 0.1 N HCl seems to help maintain solubility for final dilution of the wheat glutens.
HPLC-UV Operating Parameters:
Column: Zorbax Rx C8 (retention is too high on C18 column)
Buffer: 10 mM citric acid, 10 mM sodium octane sulfonate, adjusted to pH 3.0
Mobile phase: 85:15 buffer:acetonitrile
Flow rate: 1.0 ml/min.
Injection volume: 10 ml
Column thermostat: 40 oC (column thermostatting is necessary for ion-pair separations)
Detection wavelength: 240 nm
Spectral collection: 200 – 400 nm (look for lmax near 236 nm)
Retention time: 4.2 - 4.3 min.
Run time: 10 min.
Standard Preparation:
Stock standard was prepared in 76:24 acetonitrile: water. A check stock standard was prepared in 60:40 acetonitrile: water. Dilutions were made in either water or 0.1N HCl giving equivalent calibration curves.
Figures of Merit:
Linear range: established from 1.0 – 400 mg/ml; calibration range 1.0 – 200 mg/ml used for most of work
Reproducibility: duplicate preparations agree within 0.1 - 5% relative basis
Spike/recovery (based on spiking solid melamine powder into test matrix prior to extraction): 90 -110%.
Web page updated by mdt - April 3, 2007, 9:08 AM ET
FDA发布的气相、质谱法，包括了三聚氰胺合成时的杂质，全部测出。2007年发生的宠物粮事件后，美国FDA做了很多事，但没能引起中国国内的注意，造成今天的后果，真是可悲。政府部门都在干什么？
提供一份农业部发布的检测三聚氰胺的行业标准
毒理学杂志2008 年6 月第22 卷第3 期
J Toxicol June 2008 Vol122 No13
喂三聚氰胺后肾脏肾小管中出现了晶体。由此推断三
聚氰胺长期饲喂可能引起肾衰竭。
国内已经有采用高效液相色谱法(HPLC) 法
检测饲料和工业品的三聚氰胺的含量 ,该方法更为
灵敏,简单。
吴明礼,陈彩虹. 高效液相色谱法(HPLC) 测定单氰胺中
三聚氰胺的含量. 宁夏石油化工,2005 ,2 :24225.
辜雪英,吴小花,仇满珍. 饲料中三聚氰胺残留量高效液
相色谱测定的研究. 江西化工,2007 ,2 :18222.
帮发附件
饲料中三聚氰胺残留量高效液相色谱测定的研究.pdf (133.19k)
看看过WU君提供的资料，谢过，又明白了一点。
老美的猫阿狗阿出事的时候？用什么方法检出鉴定的Melamine？
What up？What new？
现在是用什么方法认定“重大食品安全事件”的呢？
FDA最新方法（2007-4-2）
Updated FCC Developmental Melamine Quantitation (HPLC-UV)
April 2, 2007
Sample Preparation/Extraction:
Wheat gluten: Ground in a Retsch ZM 100 centrifugal rotor mill (ring sieve 0.5 mm).
Moist pet food: Moist chunks and gravy were blended to the consistency of a gritty pudding prior to sampling.
Samples weighed into glass scintillation vials. Extract using 50:50 acetonitrile:water.
Procedure: Add indicated volume of extraction solvent (see note below) 1. Cap and vortex thoroughly, get aggressive with this step (critical due to slow dissolution rate of melamine). Sonicate 30 minutes. Filter portion of extract through 2-stage GMF-nylon (0.45 m m) filters. Dilute filtered extract 250 ml extract + 750 ml solvent 2 to maintain solubility of matrix components.
1 Wheat gluten: Extract in proportion 0.1 g to 10 ml. For melamine contents above 2% w/w, extract in proportion 0.05 g to 15 ml.
1 Moist pet food: Extract in proportion 2.0 – 2.5 g to 10 ml.
2 Solvent for final dilution may be water or 0.1 N HCl. Final dilution is necessary for compatibility with ion-pairing chromatography. We have observed some differences in behavior between the wheat gluten and pet food samples with respect to maintaining solubility during final dilution (these are most likely matrix components which fall out). 0.1 N HCl seems to help maintain solubility for final dilution of the wheat glutens.
HPLC-UV Operating Parameters:
Column: Zorbax Rx C8 (retention is too high on C18 column)
Buffer: 10 mM citric acid, 10 mM sodium octane sulfonate, adjusted to pH 3.0
Mobile phase: 85:15 buffer:acetonitrile
Flow rate: 1.0 ml/min.
Injection volume: 10 ml
Column thermostat: 40 oC (column thermostatting is necessary for ion-pair separations)
Detection wavelength: 240 nm
Spectral collection: 200 – 400 nm (look for lmax near 236 nm)
Retention time: 4.2 - 4.3 min.
Run time: 10 min.
Standard Preparation:
Stock standard was prepared in 76:24 acetonitrile: water. A check stock standard was prepared in 60:40 acetonitrile: water. Dilutions were made in either water or 0.1N HCl giving equivalent calibration curves.
Figures of Merit:
Linear range: established from 1.0 – 400 mg/ml; calibration range 1.0 – 200 mg/ml used for most of work
Reproducibility: duplicate preparations agree within 0.1 - 5% relative basis
Spike/recovery (based on spiking solid melamine powder into test matrix prior to extraction): 90 -110%.
Web page updated by mdt - April 3, 2007, 9:08 AM ET
FDA发布的气相、质谱法，包括了三聚氰胺合成时的杂质，全部测出。2007年发生的宠物粮事件后，美国FDA做了很多事，但没能引起中国国内的注意，造成今天的后果，真是可悲。政府部门都在干什么？
提供一份农业部发布的检测三聚氰胺的行业标准