本标准规定了食品中17种2,3,7,8-取代的多氯代二苯并二噁英、多氯代二苯并呋喃(PCDD/FS)和12种二噁英样多氯联苯(DL-PCBS)含量及其毒性当量(TEQ)的测定方法。（点击图片查看标准详情）
第一法 同位素稀释-气相色谱-磁式高分辨质谱法
原理:试样经提取,净化和浓缩后,采用气相色谱磁式高分辨质谱仪测定,稳定性同位素稀释法定量;以各目标化合物的毒性当量因子(TEF)与所测得的含量相乘后累加,计算样品中PCDD/Fs和DL-PCBs的TEQ。
| 水 |
| 为GB/T 6682规定的一级水 |
| 丙酮 |
| (C3H6O):农残级 |
| 正己烷 |
| (C6H14):农残级 |
| 甲苯 |
| (C7H8):农残级 |
| 环己烷 |
| (C6H12):农残级 |
| 二氯甲烷 |
| (CH2Cl2):农残级 |
| 甲醇 |
| (CH3OH):色谱级 |
| 正壬烷 |
| (C9H20):≥99% |
| 乙酸乙酯 |
| (CH3COOC2H5):农残级 |
| 硫酸钠 |
| 无水硫酸钠(Na2SO4):优级纯 |
| 硫酸 |
| 浓硫酸(H2SO4):优级纯 |
| 氢氧化钠 |
| (NaOH).优级纯 |
| 硝酸银 |
| (AgNO3):优级纯 |
| 硅藻土 |
| 提取用硅藻土:堆积密度18.0g/100mL~36.0g/100mL(如EXtrelut NT,或等效产品)。 |
| 聚苯乙烯 |
| 凝胶色谱填料:聚苯乙烯凝胶,38μm~75μm(如Bio-Beads S-X3,或等效产品)。 |
| 硅胶 |
| 75 μm~250 μm |
| 碱性氧化铝 |
| 63 μm~200μm(如EcoChrom MP Alumina B-Super l,或等效产品)。 |
| 弗罗里土 |
| 150 μm~250 μm |
| 活性炭 |
| 150μm~180μm(如CarbopackC,Supelco 10258,或等效产品)。 |
| 硅藻土 |
| 净化用硅藻土:26μm(如Celite 545 AW,Supelco 20199-U,或等效产品)。 |
| 烧瓶 |
| 250mL具塞磨口旋转烧瓶 |
| 索氏提取器 |
| – |
| 烧瓶 |
| 具塞玻璃烧瓶或玻璃三角瓶 |
| 气相色谱-高分辨质谱仪 |
| 气相色谱-磁式高分辨质谱仪(GC-HRMS) |
| 天平 |
| 感量为0.1g |
| 天平 |
| 感量为0.001g |
| 匀浆机 |
| 组织匀浆器 |
| 粉碎机 |
| – |
| 冷冻干燥机 |
| – |
| 旋转蒸发仪 |
| – |
| 氮气浓缩器 |
| – |
| 超声波清洗器 |
| – |
| 摇床 |
| – |
| 索氏提取器 |
| 配备提取套筒 |
| 快速溶剂提取仪 |
| 加速溶剂提取仪(可选) |
| 马弗炉 |
| 能够在200℃~700℃,范围内保持恒温(士10℃) |
| 烘箱 |
| 能够在105℃~250℃,范围内保持恒温(士5℃) |
| 层析柱 |
| 玻璃层析柱:带聚四氟乙烯柱塞,150mm(长)X8mm(内径),300 mm(长)X15 mm(内径)。 |
| 凝胶渗透净化系统 |
| 全自动样品净化系统:配备酸碱复合硅胶柱、碱性氧化铝柱和活性炭净化柱。 |
| 凝胶渗透色谱柱 |
| 凝胶渗透色谱柱(GPC):玻璃柱(内径15mm~20mm),内装50g S-X3凝胶,或等效全自动GPC |
| 茄形瓶 |
| – |
| 研钵 |
| 陶瓷 |
| 玻璃棉 |
| – |
| 移液管 |
| 10 mL一次性玻璃移液管 |
| 气相色谱柱 |
| 色谱柱:5%二苯基-95%二甲基聚硅氧烷柱,60mX0.25mmx0.25um,或相当者; |
| 氦气 |
| 载气:高纯氦气(>99.999%) |
第二法 同位稀释-气相色谱-三重四极杆质谱法
原理: 试样经提取、净化.分离,采用气相色谱-三重四极杆质谱联用仪测定,稳定性同位素稀释法定量;以各目标化合物的毒性当量因子(TEF)与所测得的含量相乘后累加,计算样品中PCDD/Fs和DL-PCBs的TEQ。
| 气相色谱串联质谱仪 |
| 气相色谱-三重四极杆质谱联用仪(GC-MS/MS):带电子轰击电离源(EI)或大气压化学电离源(APCI) |
附录A 17种2,3,7,8-取代PCDD/Fs和12种DL-PCBS名称、CAS号、IUPAC编号WHO规定的毒性当量因子(TEF)
| 2,3,7,8-四氯代二苯并二噁英 |
| PCDD/Fsa,2,3,7,8-TCDD,1746-01-6,WHO-2005-TEF:1.0 |
| 2,3,7,8-四氯代二苯并呋喃 |
| PCDD/Fsa,2,3,7,8-TCDF,51207-31-9,WHO-2005-TEF:0.1 |
| 1,2,3,7,8-五氯代二苯并二噁英 |
| PCDD/Fsa,1,2,3,7,8-PeCDD,40321-76-4,WHO-2005-TEF:1.0 |
| 1,2,3,7,8-五氯代二苯并呋喃 |
| PCDD/Fsa,1,2,3,7,8-PeCDF,57117-41-6,WHO-2005-TEF:0.03 |
| 2,3,4,7,8-五氯代二苯并呋喃 |
| PCDD/Fsa,2,3,4,7,8-PeCDF,57117-31-4,WHO-2005-TEF:0.3 |
| 1,2,3,4,7,8-六氯代二苯并二噁英 |
| PCDD/Fsa,1,2,3,4,7,8-HxCDD,39227-28-6,WHO-2005-TEF:0.1 |
| 1,2,3,6,7,8-六氯代二苯并二噁英 |
| PCDD/Fsa,1,2,3,6,7,8-HxCDD,57653-85-7,WHO-2005-TEF:0.1 |
| 1,2,3,7,8,9-六氯代二苯并二噁英 |
| PCDD/Fsa,1,2,3,7,8,9-HxCDD,19408-74-3,WHO-2005-TEF:0.1 |
| 1,2,3,4,7,8-六氯代二苯并呋喃 |
| PCDD/Fsa,1,2,3,4,7,8-HxCDF,70648-26-9,WHO-2005-TEF:0.1 |
| 1,2,3,6,7,8-六氯代二苯并呋喃 |
| PCDD/Fsa,1,2,3,6,7,8-HxCDF,57117-44-9,WHO-2005-TEF:0.1 |
| 1,2,3,7,8,9-六氯代二苯并呋喃 |
| PCDD/Fsa,1,2,3,7,8,9-HxCDF,72918-21-9 |
| 2,3,4,6,7,8-六氯代二苯并呋喃 |
| PCDD/Fsa,2,3,4,6,7,8-HxCDF,60851-34-5 |
| 1,2,3,4,6,7,8-七氯代二苯并二噁英 |
| PCDD/Fsa,1,2,3,4,6,7,8-HpCDD,35822-46-9 |
| 1,2,3,4,6,7,8-七氯二苯并呋喃 |
| PCDD/Fsa,1,2,3,4,6,7,8-HpCDF,67562-39-4 |
| 1,2,3,4,7,8,9-七氯二苯并呋喃 |
| PCDD/Fsa,1,2,3,4,7,8,9-HpCDF,55673-89-7 |
| 八氯代二苯并二噁英 |
| PCDD/Fsa,OCDD,3268-87-9 |
| 八氯代二苯并呋喃 |
| PCDD/Fsa,OCDF,39001-02-0 |
| 3,3’，4,4’-四氯联苯 |
| 3,3’,4,4’-TeCB,77,32598-13-3 |
| 3,4,4’,5-四氯联苯 |
| 3,4,4’,5-TeCB,81,70362-50-4 |
| 2,3,3’,4,4’-五氯联苯 |
| PCBsb,2,3,3’,4,4’-PePCB,,32598-14-4,105 |
| 2,3,4,4’,5-五氯联苯 |
| PCBsb,2,3,4,4’,5-PePCB,74472-37-0,114 |
| 2,3’,4,4’,5-五氯联苯 |
| PCBsb,2,3’,4,4’,5-PePCB,31508-00-6,118 |
| 2’,3,4,4’,5-五氯联苯 |
| PCBsb,2’,3,4,4’,5-PePCB,65510-44-3,123 |
| 3,3’，4,4’，5-五氯联苯 |
| PCBsb,3,3’,4,4’,5-PePCB,57465-28-8,126 |
| 2,3,3’,4,4’,5-六氯联苯 |
| PCBsb,2,3,3’,4,4’,5-HxPCB,38380-08-4,156 |
| 2,3,3’,4,4’,5’-六氯联苯 |
| 2,3,3’,4,4’,5’-HxCB,157,C12H4Cl6,69782-90-7 |
| 2,3’,4,4’,5,5’-六氯联苯 |
| PCBsb,2,3’,4,4’,5,5’-HxPCB,52663-72-6,167 |
| 3,3’，4,4’，5,5’-六氯联苯 |
| PCBsb,3,3’;,4,4’,5,5’-HxPCB,32774-16-6,169 |
| 2,3,3’，4,4’，5,5’-七氯联苯 |
| PCBsb,2,3,3’4,4’,5,5’-HPCB,39635-31-9,189 |
| 1,2,3,4-四氯代二苯并二噁英 |
| 1,2,3,4-TCDD,30746-58-8 |
| 1,2,3,7-四氯代二苯并二噁英 |
| 1,2,3,7-TCDD,67028-18-6 |
| 1,2,3,8-四氯二苯并-对-二噁英 |
| 53555-02-5,1,2,3,8-Tetrachlorodibenzo-p-dioxin |
| 2,3,7,8-四氯代二苯并二噁英 |
| PCDD/Fsa,2,3,7,8-TCDD,1746-01-6 |
| 1,2,3,9-四氯代二苯并二噁英 |
| 1,2,3,9-TCDD,71669-26-6 |
| 1,2,3,4,7,8-六氯代二苯并呋喃 |
| PCDD/Fsa,1,2,3,4,7,8-HxCDF,70648-26-9 |
| 1,2,3,6,7,8-六氯代二苯并呋喃 |
| PCDD/Fsa,1,2,3,6,7,8-HxCDF,57117-44-9 |
| 13C12-2,3,7,8-四氯代二苯并二噁英 |
| 同位素标记的PCDD/Fs,13C12-2,3,7,8-TCDD,76523-40-5 |
| 13C12-2,3,7,8-四氯代二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-2,3,7,8-TCDF,89059-46-1 |
| 13C12-1,2,3,7,8-五氯代二苯并二噁英 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,7,8-PeCDD,109719-79-1 |
| 13C12-1,2,3,7,8-五氯代二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,7,8-PeCDF,109719-77-9 |
| 13C12-2,3,4,7,8-五氯代二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-2,3,4,7,8-PeCDF,116843-02-8 |
| 13C12-1,2,3,4,7,8-六氯代二苯并二噁英 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,4,7,8-HxCDD,109719-80-4 |
| 13C12-1,2,3,6,7,8-六氯代二苯并二噁英 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,6,7,8-HxCDD,109719-81-5 |
| 13C12-1,2,3,4,7,8-六氯代二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,4,7,8-HxCDF,114423-98-2 |
| 13C12-1,2,3,6,7,8-六氯代二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,6,7,8-HxCDF,116843-03-9 |
| 13C12-1,2,3,7,8,9-六氯代二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,7,8,9-HxCDF,116843-04-0 |
| 13C12-2,3,4,6,7,8-六氯代二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-2,3,4,6,7,8-HxCDF,116843-05-1 |
| 13C12-1,2,3,4,6,7,8-七氯代二苯并二噁英 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,4,6,7,8-HpCDD,109719-83-7 |
| 13C12-1,2,3,4,6,7,8-七氯二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,4,6,7,8-HpCDF,109719-84-8 |
| 13C12-1,2,3,4,7,8,9-七氯二苯并呋喃 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,4,7,8,9-HpCDF,109719-94-0 |
| 13C12-八氯代二苯并二噁英 |
| 同位素标记的PCDD/Fs,13C12-OCDD,114423-97-1 |
| 13C12-1,2,3,4-四氯代二苯并二噁英 |
| 13C-1,2,3,4-TCDD ,114423-99-3 |
| 13C12-1,2,3,7,8,9-六氯代二苯并二噁英 |
| 同位素标记的PCDD/Fs,13C12-1,2,3,7,8,9-HxCDD,109719-82-6 |
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