美国农业部食品安全监督服务局发布的牛肉中氟尼辛残留的检查方法 处理样品用的是多管涡旋振荡器(muti tube vortexer) http://www.fsis.usda.gov/PDF/CLG_FLX_4_03.pdf 节选部分: B. EQUIPMENT 1. Apparatus a. Blender - Model No. 51BL31, Waring Inc. b. Balance, analytical - Sensitive to 0.1 mg, Model No. A120S, Sartorius. c. Balance, top loading - Sensitive to 0.01 g, Model No. E83200D, Shimadzu. d. Centrifuge - Capable of 700 x g and holding 50 mL glass centrifuge tubes, Model No. Centra-7R, International Equipment Company. e. Evaporator - Nitrogen evaporator, N-Evap®, Model No. 111, Organomation. f. Glass centrifuge tube - Pyrex® round-bottom screw-cap, 29 mm, 50 mL centrifuge tube, Cat. No. 21023-401, VWR. g. Polypropylene centrifuge tubes - 50 mL conical, with closures, Cat. No. 352070, Blue Max. h. Glass disposable Pasteur pipettes - 9-inch, Cat. No. 14672-380, VWR. i. Glass volumetric flask - Class A, 10, 50, 100, and 1000 mL, Kimax. j. Glass graduated cylinder - 500 mL. k. Heating Block - Pierce Reach-Therm™ III (Cat. No. 18935 H, Pierce) with three aluminum heating blocks holding at least twelve 29 mm 50 mL centrifuge tubes. The heating block is custom drilled from a blank aluminum block (Cat. No. 18810 H, Pierce). l. pH meter - Capable of 0.01 pH unit sensitivity, Model No. 340 pH meter, Corning. m. Pipettes - Automatic pipettors capable of accuray delivering 300 μL to 5 mL volume. n. Repipetters - Bottle top dispensers of appropriate volume. o. Spatula - stainless steel or plastic. p. Test tube racks - for 15 and 50 mL tubes. q. Solid Phase Extraction Vacuum Manifold - Cat. No. 57030-U, Supelco. r. Trap for SPE Vacuum Manifold - Side arm flask with tubing, Cat. No. 57120-U, Supelco. s. SCX Cartridges - Benzenesulfonic acid cation exchange (SCX), 500-mg/3 mL, Cat. No. 2323, Applied Separations, Allentown, PA. t. Reservoirs - Empty polypropylene SPE tubes (no frits) 60 mL, Cat. No. 57022, Supelco. u. Cartridge Adapters - For 3 mL tubes, Cat. No. 57020-U, Supelco. v. Disposable glass culture tubes - 15 mL, 16 x 100 mm, Cat. No. 73500 16100, Kimble. w. Vortexer - Vortexer-2, and multi-tube vortexer, Cat. No. 58816-115, x. Phase Filtration Apparatus - Cat. No. 58062-U, Supelco. y. Membrane Filter Disks - 0.45 μm pore size, 47 mm, nylon, HPLC phase membrane filter, Cat. No. HNWP 047 00, Fisher. z. Whatman Mini-Uniprep syringeless filters - Standard, PTFE, 0.45 μm, Cat. No. 09-923-28, Fisher.
2. Instrumentation LC/ESI-MS/MS System a. Pumps - Two Varian Prostar model 210 pumps, Master and Slave. b. Autosampler with column heating compartment - Varian Prostar model 410 autosampler. c. Source - Varian Electrospray ionization. d. Detector - Model 1200L quadrupole MS/MS, Varian. e. Analytical Column - Eclipse XDB-C18 2.1 x 150 mm, 5 μm, Cat. No. 993700-902, Agilent. f. Guard Column - Brownlee cartridge column, RPI8, 7 μm, 3.2 x 15 mm, Cat. No. 0711-0092 and NewGuard holder, Cat. No. 0715-0001, Chrom Tech. |