本標準規(guī)定了食品中17種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種二噁英樣多氯聯(lián)苯(DL-PCBS)含量及其毒性當量(TEQ)的測定方法。（點擊圖片查看標準詳情）
第一法 同位素稀釋-氣相色譜-磁式高分辨質(zhì)譜法
原理:試樣經(jīng)提取,凈化和濃縮后,采用氣相色譜磁式高分辨質(zhì)譜儀測定,穩(wěn)定性同位素稀釋法定量;以各目標化合物的毒性當量因子(TEF)與所測得的含量相乘后累加,計算樣品中PCDD/Fs和DL-PCBs的TEQ。
| 水 |
| 為GB/T 6682規(guī)定的一級水 |
| 丙酮 |
| (C3H6O):農(nóng)殘級 |
| 正己烷 |
| (C6H14):農(nóng)殘級 |
| 甲苯 |
| (C7H8):農(nóng)殘級 |
| 環(huán)己烷 |
| (C6H12):農(nóng)殘級 |
| 二氯甲烷 |
| (CH2Cl2):農(nóng)殘級 |
| 甲醇 |
| (CH3OH):色譜級 |
| 正壬烷 |
| (C9H20):≥99% |
| 乙酸乙酯 |
| (CH3COOC2H5):農(nóng)殘級 |
| 硫酸鈉 |
| 無水硫酸鈉(Na2SO4):優(yōu)級純 |
| 硫酸 |
| 濃硫酸(H2SO4):優(yōu)級純 |
| 氫氧化鈉 |
| (NaOH).優(yōu)級純 |
| 硝酸銀 |
| (AgNO3):優(yōu)級純 |
| 硅藻土 |
| 提取用硅藻土:堆積密度18.0g/100mL~36.0g/100mL(如EXtrelut NT,或等效產(chǎn)品)。 |
| 聚苯乙烯 |
| 凝膠色譜填料:聚苯乙烯凝膠,38μm~75μm(如Bio-Beads S-X3,或等效產(chǎn)品)。 |
| 硅膠 |
| 75 μm~250 μm |
| 堿性氧化鋁 |
| 63 μm~200μm(如EcoChrom MP Alumina B-Super l,或等效產(chǎn)品)。 |
| 弗羅里土 |
| 150 μm~250 μm |
| 活性炭 |
| 150μm~180μm(如CarbopackC,Supelco 10258,或等效產(chǎn)品)。 |
| 硅藻土 |
| 凈化用硅藻土:26μm(如Celite 545 AW,Supelco 20199-U,或等效產(chǎn)品)。 |
| 燒瓶 |
| 250mL具塞磨口旋轉(zhuǎn)燒瓶 |
| 索氏提取器 |
| – |
| 燒瓶 |
| 具塞玻璃燒瓶或玻璃三角瓶 |
| 氣相色譜-高分辨質(zhì)譜儀 |
| 氣相色譜-磁式高分辨質(zhì)譜儀(GC-HRMS) |
| 天平 |
| 感量為0.1g |
| 天平 |
| 感量為0.001g |
| 勻漿機 |
| 組織勻漿器 |
| 粉碎機 |
| – |
| 冷凍干燥機 |
| – |
| 旋轉(zhuǎn)蒸發(fā)儀 |
| – |
| 氮氣濃縮器 |
| – |
| 超聲波清洗器 |
| – |
| 搖床 |
| – |
| 索氏提取器 |
| 配備提取套筒 |
| 快速溶劑提取儀 |
| 加速溶劑提取儀(可選) |
| 馬弗爐 |
| 能夠在200℃~700℃,范圍內(nèi)保持恒溫(士10℃) |
| 烘箱 |
| 能夠在105℃~250℃,范圍內(nèi)保持恒溫(士5℃) |
| 層析柱 |
| 玻璃層析柱:帶聚四氟乙烯柱塞,150mm(長)X8mm(內(nèi)徑),300 mm(長)X15 mm(內(nèi)徑)。 |
| 凝膠滲透凈化系統(tǒng) |
| 全自動樣品凈化系統(tǒng):配備酸堿復合硅膠柱、堿性氧化鋁柱和活性炭凈化柱。 |
| 凝膠滲透色譜柱 |
| 凝膠滲透色譜柱(GPC):玻璃柱(內(nèi)徑15mm~20mm),內(nèi)裝50g S-X3凝膠,或等效全自動GPC |
| 茄形瓶 |
| – |
| 研缽 |
| 陶瓷 |
| 玻璃棉 |
| – |
| 移液管 |
| 10 mL一次性玻璃移液管 |
| 氣相色譜柱 |
| 色譜柱:5%二苯基-95%二甲基聚硅氧烷柱,60mX0.25mmx0.25um,或相當者; |
| 氦氣 |
| 載氣:高純氦氣(>99.999%) |
第二法 同位稀釋-氣相色譜-三重四極桿質(zhì)譜法
原理: ?試樣經(jīng)提取、凈化.分離,采用氣相色譜-三重四極桿質(zhì)譜聯(lián)用儀測定,穩(wěn)定性同位素稀釋法定量;以各目標化合物的毒性當量因子(TEF)與所測得的含量相乘后累加,計算樣品中PCDD/Fs和DL-PCBs的TEQ。
| 氣相色譜串聯(lián)質(zhì)譜儀 |
| 氣相色譜-三重四極桿質(zhì)譜聯(lián)用儀(GC-MS/MS):帶電子轟擊電離源(EI)或大氣壓化學電離源(APCI) |
附錄A 17種2,3,7,8-取代PCDD/Fs和12種DL-PCBS名稱、CAS號、IUPAC編號WHO規(guī)定的毒性當量因子(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’-四氯聯(lián)苯 |
| 3,3’,4,4’-TeCB,77,32598-13-3 |
| 3,4,4’,5-四氯聯(lián)苯 |
| 3,4,4’,5-TeCB,81,70362-50-4 |
| 2,3,3’,4,4’-五氯聯(lián)苯 |
| PCBsb,2,3,3’,4,4’-PePCB,,32598-14-4,105 |
| 2,3,4,4’,5-五氯聯(lián)苯 |
| PCBsb,2,3,4,4’,5-PePCB,74472-37-0,114 |
| 2,3’,4,4’,5-五氯聯(lián)苯 |
| PCBsb,2,3’,4,4’,5-PePCB,31508-00-6,118 |
| 2’,3,4,4’,5-五氯聯(lián)苯 |
| PCBsb,2’,3,4,4’,5-PePCB,65510-44-3,123 |
| 3,3’，4,4’，5-五氯聯(lián)苯 |
| PCBsb,3,3’,4,4’,5-PePCB,57465-28-8,126 |
| 2,3,3’,4,4’,5-六氯聯(lián)苯 |
| PCBsb,2,3,3’,4,4’,5-HxPCB,38380-08-4,156 |
| 2,3,3’,4,4’,5’-六氯聯(lián)苯 |
| 2,3,3’,4,4’,5’-HxCB,157,C12H4Cl6,69782-90-7 |
| 2,3’,4,4’,5,5’-六氯聯(lián)苯 |
| PCBsb,2,3’,4,4’,5,5’-HxPCB,52663-72-6,167 |
| 3,3’，4,4’，5,5’-六氯聯(lián)苯 |
| PCBsb,3,3’;,4,4’,5,5’-HxPCB,32774-16-6,169 |
| 2,3,3’，4,4’，5,5’-七氯聯(lián)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-對-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 |
| 同位素標記的PCDD/Fs,13C12-2,3,7,8-TCDD,76523-40-5 |
| 13C12-2,3,7,8-四氯代二苯并呋喃 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的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 |
| 同位素標記的PCDD/Fs,13C12-1,2,3,4,7,8,9-HpCDF,109719-94-0 |
| 13C12-八氯代二苯并二噁英 |
| 同位素標記的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 |
| 同位素標記的PCDD/Fs,13C12-1,2,3,7,8,9-HxCDD,109719-82-6 |
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