HPLC实验报告.doc

1. , ( endocrine disrupting chemicals, edcs) , , ( ) , edcs ( ngl-1 ), edcs edcs -edcs gc- ms hplc, , (elisa), gc - ms hplcgc- ms , , (spe) , (hplc), , ee2, 2. 2.1. lc-20arf-10axlinertsil ods-sp-c18150mm4.6mm,5mhp-6019-12 spe6ml2g/ml,ee2hplcc182.2. 2g/ml ee2 0.25ml0.5ml1ml2ml5ml7.5ml10ml2g/ml ee2 0.5ml100ml2.3. c18 spe6ml0.2gc182.4. inertsil ods-sp-c18150mm4.6mm,5m/25:30:451.0ml/min4020l280nm310nm2.5. 100ml58ml/min5.00ml5.00mlc18 spe5.00ml3.0min10.00ml4050%2.00ml0.22mhplc/fld 3 3.1 0.05g/ml0.1g/ml0.2g/ml0.4g/ml1g/ml1. 5g/mlee2hplc/fld1ee2- 1 1yxg/ml1072yx,g/mly=4.6106x+2557.8r2=1.0000 3.2 hplc/fld17682770.3838g/mlw% w%=3.3 1c18 spe2344 (spe) , (hplc), , ee20.9995ee276.76%1 , , , . -a. , 2006, 25(9): 2729 0.3838g/ml?2ml2g/ml?0.5ml?100%?76.76%2 , , , . hplc-ms/ms. , 2011, 30(12): 8123 , , , . . , 2009, 28(11): 41444 , , , . spe-hplc-ms/ms., 2011, 30(3): 4244275 , , , . . , 2011, 27 (5): 86926 , , . 5 . , 2008, 25 (5): 4384417 , , , . a. , 2006, 34(10): 141914228 , , . . , 2004, 11(2):3603619 . . , 1997, 13 (4) : 251-252 10, . . , 2005, 3(5): 310 11, , . . , 2007,26(2):288294 1 2 3 hplc 80% 1 hplc 2 3 hplc3m5m7m10m1m10mhplc50000/m160000/m100-300mm 4 hplc 5 11 1. 2 2 1 2 35 1 ph 2 3 4 55 6 7 hplc 1. hplc 2. 3. 1200hplc10l (ph=3)1. ph=3 2. 1 3. 1200hplc 4. 5. 10l5l 6. 7. 1. lc2. 3. a 0.0 1.000ml/min b 0.0 91bar c 0.0 d 0.05. 5l(l)(h)(n) n = l / h n = 16 ( tr / wb ) 2 = 5.54 ( tr / y1/2 ) 2 tr =2.437 min = 146.22s y1/2 = 2.354(0.1375min / 4 ) = 4.855125 s n = 5.54 ( tr / y1/2 ) 2 =5025 ()1.188min1.420min1.531min1.816min, 2.437min3.196min 12 113 2014561. hplc2. 3. hplc hplc10l6:42,2-4-4-bapp1. 6:42. 13. (50mgbapp50ml)4. 5. 25ml5mlbappbapp6. 7. y=701.393x+14.513y=30830.8x-796.0712.983min0.3326min1619.79114mau93.3238104mau*s9.33238104mau*sc=3.05mg/ml1619.79114mauc=2.29mg/ml2.29mg/ml1. 2. 3. 4. 5. c-186. 5%95%407. ()2009* 2011 5 301234 , , , : a0.9508 g 5 mmol/l+ 1.0640 gph=3-41lb30%b+70%acnwsil c18 4.6250mm5 m239 nm: y = 4495951 x +18978.83 , r = 0.9999693, 0.17110.0 mg/l, 0.12 mg/l, 96.34 % (rsd =8. 76)84.86 % (rsd = 7.21) 104.29 % (rsd = 7.63) 95.31 %(rsd = 4.39) 89.25 % (rsd = 3.88) 92.59 % (rsd = 5.27) ; ; (melamine) c3h6n6iupac1,3,5-2,4,6-, 1 9. 1g/l 16666.251/5, , 20089, 2 , 3 15-20%10-20%16%18%2.88%66.6%15123100g0.10.625%1g(ml)100mltüv(fcc)hplc-uvhplc/ms(, , ), . ny/t 13722007 4 , 5 , gb/t22388-2008-/-elisa-1hplc)2mg/kg10mg/kg80%110%10%2-gc-msgc-ms/mssimmrmgc-ms0.05mg/kg2mg/kg70%110%10%gc-ms/ms0.005mg/kg1mg/kg90%105%10%3-/lc-ms/ms-/0.01mg/kg0.5mg/