食品中动物用药残留量检验方法四环霉素类抗生素之检验

1、Method of Test for Veterinary Drug Residues in Foods Test of Tetracyclines1. A dA VdAA(tetracycline, TC)?Bm(oxytetracycline, OTC)?B(chlortetracycline, CTC)m(Doxycycline) C ¤2. hR(high performance liquid chromatography, HPLC)?2.1 ?m.2.1.1hR°2.1.1.1E o i380 nmA o?g i520 nm(Fluorescencedetect

2、or)?C2.1.1.2 hRLuna C18 (2)?A 5 m?A4.6 mm × 25 cmPC.2.1.2§(Homogenizer)?C.2.1.3V±(Vortex mixer)?C.2.1.4Ym(Rotary evaporator)?C2.1.5?(Centrifuge)?.2.2?hRACBuBL BfcB(imidazole)?BLBNa2-EDTA (disodium ethylenediaminetetraacetate)?BvBBBuFBBmmC2.3?2.3.1?1000 mL?C2.3.2 .C18 T500 mg?A Oasis H

3、LB PC.2.3.3 ?Y100 mL?C2.3.4?o0.22Bm?0.45 Am?polyvinylidene difluoride C2.3.5?eq100 mL?C2.3.6lqLom¤(Molecular weight cutoff filter)Centricon YM-30PC2.4?s2.4.1 0.1M fcfc1.9 g?AH100 mL?C2.4.2 0.2M CBuCBu2.84 g?AH100 mL?C2.4.3pH4.0 MacIlvaine ?wq0.1 M fc615 mL M 0.2 M C Bu385 mL VAnpH C2.4.4t §

4、;0.01 M Na2-EDTApH 4.0 MacIlvaine w1Na2-EDTA 3.36 g?AHpH 4.0 MacIlvaine w1,000 mLC2.4.5pH7.2 ?w68.08 g?AL10.72 gNa2-EDTA 0.37 g?A Hhl800 mLA LpH7.2 Hhlwe1,000 mLC2.4.60.05 N ?q4.17 mL?AHhl1,000 mL?C2.52swPH77? 23 (v/v)V ¤A g 0.45moLoAoC2.6tsBB mm10 mg?ATwAOHwe100mLAAH0.05 N 0.011.0 g/mLAC2.7 C1

5、8TH3 mL2 mL M Ayt1.5 mL/min?C2.8sà2.8.1 ×NBA5 g?A TwA t0.01M Na2-EDTApH 4.0 MacIlvaine w15 mL RVA3,000 rpm15CAv10 mL 2V¤ ?A?3,000órpm15 AhABCNhwC18 TAyAH 5%￥2 mL M A AH10 mL R CR40DYA dH0.05 N we1 mL?Ag0.22moLoC2.8.2 ¨1 mLA t0.01M Na2-EDTA pH 4.0 MacIlvaine w3mL RVA1 mL lqLomA3,000 rpm Lo60 AoC2.9 ?OtqwTq100 AL?OhRACihRA NPoipdOACpDtq(ppm)?tq(ppm) =C×VMC?uDo×( g/mL)2V?gwen(mL)M?Rq(g)hRwhRLuna C18(2)A5 m?A4.6 mm × 25 c