KS H ISO 22634-2012 Cigarettes－Determination of benzo[a]pyrene in cigarette mainstream smoke－Method using gas chromatography mass spectrometry《香烟 香烟主流烟气中苯并[a]芘的测定 气相色谱分析 质谱分析法》.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS H ISO 22634 / KS H ISO 22634:2012 2012 9 19 http:/www.kats.go.krKS H ISO 22634:2012 : ( ) ( ) () () ( ) : (ISO/TC126) () ( ) () KT&G () KT&G () () ( ) KT&G : (http:/www.standard.go.kr) ： ：2012 9 19 2012-0452 ： ：(ISO/TC126) ( 02-509-7266) (http:/www.kats.g

2、o.kr). 10 5 , . KS H ISO 22634:2012 i ii . iii 1 1 2 1 3 1 4 2 5 2 6 .3 6.1 1 BaP .3 6.2 2 BaP .3 6.3 BaP-d12 3 6.4 BaP-d12 3 6.5 .3 6.6 .3 7 .3 7.1 3 7.2 .3 7.3 .3 7.4 (clean-up) .4 8 5 8.1 GC-MS .5 8.2 .5 8.3 BaP 5 8.4 .5 9 6 10 .6 10.1 6 10.2 .6 10.3 .7 10.4 .7 10.5 7 A( ) 8 10 KS H ISO 22634:201

3、2 ii ISO(the International Organization for Standardization) (ISO ) . ISO . . ISO . ISO (IEC) . ISO/IEC , 2 . . . 75 % . . ISO . ISO/TC 126, . KS H ISO 22634:2012 iii 2008 1 ISO 22634, Cigarettes Determination of benzoapyrene in cigarette mainstream smoke Method using gas chromatography/mass spectro

4、metry . 1999 2003 CORESTA1) (BaP) . , . (HPLC)2) - (GC-MS)3) . BaP . HPLC . , . GC-MS , . , . ISO . . . ( ) , . . , ISO . 1) CORESTA： Cooperation Centre for Scientific Research Relative to Tobacco 2) High performance liquid chromatography 3) Gas chromatography-mass spectrometry KS H ISO 22634:2012 /

5、 Cigarettes Determination of benzoapyrene in cigarette mainstream smoke Method using gas chromatography/mass spectrometry 1 (benzoapyrene, BaP) . KS H ISO 3308 . 2 . . ( ) . KS H ISO 3308, KS H ISO 4387, KS H ISO 8243, KS M ISO 3696, 3 KS H ISO 4387 / cyclohexyl solid phase extraction(CH SPE) cartri

6、dge , BaP . / BaP KS H ISO 22634:2012 2 4 . 4.1 , KS H ISO 3308 KS H ISO 4387 4.2 , . (single ion monitoring, SIM) . . . 4.3 , (methylphenyl, 5 %) (polysiloxane) . , 30 m, 0.25 mm , 0.25 m . 4.4 4.5 . 4.6 (cyclohexyl solid phase extraction, CH-SPE) , (phase)： . 6 mL, 1 g . 4.7 (gas tight syringe), 2

7、5 L, 100 L, 250 L 1 000 L . 4.8 , , . . 5 . 5.1 5.2 , KS M ISO 3696 2 . 5.3 5.4 5.5 (Benzoapyrene, BaP) 5.6 -d12(Benzoapyrene-d12, BaP-d12) - d12 . . KS H ISO 22634:2012 3 6 6.1 1 BaP 10 mg BaP 0.01 mg 10 mL . 6.2 2 BaP 1 BaP (6.1) 1 mL 100 mL . 6.3 BaP-d12 10 mg BaP-d12 0.01 mg 10 mL . 6.4 BaP-d12

8、BaP-d12 (6.3) 100 L 100 mL . 1 g/mL . 6.5 6 . , 2 BaP 10 L 2 000 L 100 mL , 20 L BaP-d12 (6.3) . BaP-d12 0.2 g/mL , BaP 1 ng/mL 200 ng/mL . 6.6 (6.1 6.5) 18 6 . 7 7.1 KS H ISO 8243 . 7.2 KS H ISO 4387 . 44 mm 10 , 92 mm 20 . 44 mm 150 mg (TPM) , 92 mm 600 mg . . 44 mm 10 mg, 92 mm 20 mg TPM . 7.3 KS

9、 H ISO 22634:2012 4 7.3.1 ( ) . 7.3.2 (44 mm 100 mL, 92 mm 200 mL) . 7.3.3 44 mm , 20 mL BaP-d12 (6.4) 200 L . 92 mm , 50 mL BaP-d12 (6.4) 400 L . 7.3.4 , (glass suction filter) . 7.3.5 44 mm 15 mL , 92 mm 25 mL . , 44 mm 40 mL , 92 mm 80 mL . . 7.3.6 7.3.5 . 40 mL . (7.4.2 ) . 7.3.7 60 % 40 % . , 7

10、.3.6 40 mL , 60 mL . 7.4 (clean-up) 7.4.1 CH SPE 10 mL , (60： 40 ) 10 mL (pre-condition) . 7.4.2 CH SPE 2 mL/min( 1 ) . (60： 40 ) 10 mL . 30 . 7.4.3 15 mL (5.3) . 7.4.4 (4.4) 0.5 mL . 1 mL . 7.4.2 7.4.3 , 7.4.4 . 1 mL . , 7.4.3 . 7.4.5 (polytetrafluoroethylene, PTFE) (septum) . KS H ISO 22634:2012 5

11、 8 8.1 GC-MS ： 290 ： (constant flow) ： 0.9 mL/min ： 1 L ： 80 3 5 /min 290 . 290 20 (transfer line temp)： 270 ： 230 ： BaP： m/z 252( ) 250( ) BaP-d12： m/z 264( ) 260( ) BaP BaP-d12 . A . 8.2 (6.5) GC-MS . BaP BaP-d12 . BaP BaP BaP BaP-d12 . 0 . 10 1 (6.5) 15 % . 8.3 BaP BaP BaP-d12 , BaP BaP . BaP BaP

12、-d12 . GC-MS . , . 8.4 BaP , m , . ceVnVVCm= , C ： BaP (ng/mL) V ： (mL)(V 1 mL) Ve： (7.3.5) n ： KS H ISO 22634:2012 6 Vc： (7.3.6) 9 2R4F( ) 7 , 13 2003 , , (r) (R) . 2 20 1 (r) . 2 20 1 (R) . 7 1 . 1 BaP(ng/ ) r R 2R4F 7.28 1.27 2.52 A 1.81 0.49 1.01 B 5.27 1.06 2.52 C 6.54 1.11 2.21 D 7.76 1.47 2.8

13、8 E 8.71 1.39 2.72 F 14.07 2.26 5.94 10 10.1 , . . 10.2 10.5 . 10.2 . . KS H ISO 22634:2012 7 ( ) ( ) (overwrap) 10.3 ( , ) 10.4 ( ) (%) (kPa) 10.5 . . BaP ( ), 0.1 ng KS H ISO 22634:2012 8 A ( ) A.1 X ( ) Y KS H ISO 22634:2012 9 4.3 8.1 BaP BaP-d12 40 45 . 252 264 . 40 65 . BaP BaP-d12 . KS H ISO 2

14、2634:2012 10 KS H ISO 3402, - - / 153787 1 92 3(13) (02)26240114 (02)262401489 http:/ Korean Agency for Technology and Standards http:/www.kats.go.kr KS H ISO 22634:2012 KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS CigarettesDetermination of benzoapyrene in cigarette mainstream smokeMethod using gas chromatography/mass spectrometry ICS 65.160