- 518045 - GC-MS RSD 14% 83. 6% ~ 104. 1% 10 S /N = 10 DINP DIDP DMPP 0. 2 0. 2 0. 1 mg /kg 0. 05 mg - O658 A 0254-508X 2013 03-0024-06 Simultaneous Determination of Phthalate Plasticizers in Coated Papers by Gas Chromatography-tandem Mass Spectrometry Coupled with Microwave-assisted Extraction WANG Cheng-yun * XU Rong YANG Zuo-jun WU Tou-ming XIE Tang-tang ZHU Nai-qing Shenzhen Entry-exit Inspection and Quarantine Bureau Shenzhen Guangdong Province 518045 * E-mail wangchengyun2009@ 126. com Abstract Phthalate plasticizers in coated papers were microwave-assisted extracted using acetone as the extraction solvent and then were analyzed by gas chromatography-tandem mass spectrometry GC-MS. Therefore an effective method was established to determine simultaneously the contents of phthalate plasticizers in coated papers. The relative standard deviation RSD of the proposed method was less than 14% while the average spike recoveries varied from 83. 6% to 104. 1%. The quantification limits S /N = 10 were 0. 2 0. 2 and 0. 1 mg / kg for DINP DIDP and DMPP respectively. The limits of quantification S /N = 10 were all less than 0. 05 mg /kg for other phthalate plasticizers. The proposed method was successfully applied to the determination of phthalate plasticizers in coated papers and the results showed that various phthalate plasticizers existed in some commercial coated papers. Key words coated paper phthalate gas chromatography-tandem mass spectrometry microwave-assisted extraction 12 1-3 13-15 - GC-MS 4-5 16-18 6-11 12 - GC-MS 2012-12-06 24 China Pulp & Paper Vol. 32 No. 3 2013
1 1. 1 MAR5 CEM Agilent 8 DMPP 12. 70 251 167 149 * 30 5 75 9 DEOEP 13. 18 207 176 191 * 149 20 5 75 10 DAP 13. 60 237 219 149 * 149 5 5 75 11 DHXP 16. 33 251 233 149 * 149 5 5 75 12 BBP 16. 45 238 206 104 149 * 35 5 75 13 DBOEP 18. 34 193 176 149 * 149 20 5 75 14 DCHP 19. 14 249 167 149 * 30 5 75 7890A-7000B Agilent 1 min 15 /min 210 2 min Heidolph 4003 Heidolph 5 /min 240 5 min 5 /min 250 5 min 25 /min 300 DMP 4 min 1 μl DEP DALP 280 260 DPRP > 99. 999% 1. 2 ml /min DIBP DBP 5. 0 min 2- DMOEP 4-1. 4. 2-2- DMPP 2-150 230 DEOEP DAP EI 70 ev DHXP 1. 5 ml /min 2. 25 ml /min BBP 2- DBO- MRM EP DCHP 1 DHP 2-1 DEHP DNOP DINP /min m z m z /V /ms DIDP 1 DMP 6. 94 194 163 163 77 * 5 25 150 DNP 2 DEP 8. 07 222 177 149 * 40 5 50 99. 0% 3 DALP 9. 23 189 132 41 104 * 10 5 50 4 DPRP 9. 44 209 191 149 * 149 5 5 50 5 DIBP 10. 25 223 205 149 * 149 5 5 75 6 DBP 11. 25 223 205 149 * 149 5 5 75 TEDIA 7 DMOEP 11. 70 207 176 59 * 149 5 5 75 0. 45 μm Membrana 1. 2 1. 3 0. 5 g 15 ml 15 DHP 19. 49 265 167 149 * 35 5 75 16 DEHP 19. 67 279 167 149 * 35 5 75 17 DNOP 24. 02 279 149 * 71 5 5 150 20 24. 20 ~ 293 293 149 * 167 18 DINP 5 5 40 40 28. 30 293 71 2 min 15 ml 25 ml 0. 45 μm GC-MS 2013 32 3 1. 4 1. 4. 1 Agilent HP-5MS 30 m 0. 25 mm 0. 25 μm 90 28. 50 ~ 307 307 149 * 167 19 DIDP 5 5 40 40 31. 20 307 71 20 DNP 29. 40 293 167 149 * 5 5 40 * 25
2 2. 1 DIDP 19 17 2 mg /kg DMP DEP DIBP DBP DEHP 13 15 min 30 min 1 /3 260 50 14 10 ~ 20 20 - - 6 8 10 12 17-20 - - - 2 1-1 1-1 1-1 1-1 3-1 1 17 1 1 DINP 18 DIDP 19 DNP 20 36 11 32 67 1202 47 34 38 83 2145 36 40 28 64 1750 30 21 22 56 1590-24 39 26 55 1642 20 26 17 47 204-2 1 20 32 40 61 1624-1 1 15 20 20 98 1212 20 27 25 63 1018 15 27 22 52 1265 12 20 17 38 1516 14 17 26 88 1305 1 1 13 20 28 59 1428 8 8 17 18 167 1 1 7 8 24 51 1474 1 3 6 9 16 62 1058-1 1 4 4 21 69 1171 2 2 2. 2 20 1 2. 3 c A r 0. 9960 3 S /N = 10 1 1 3 26 China Pulp & Paper Vol. 32 No. 3 2013
3 /min /ng ml - 1 /ng g - 1 1 DMP 6. 94 15. 6 ~ 936 A = 3515. 4c + 80551 0. 9994 10 2 DEP 8. 07 13. 7 ~ 273 A = 1972. 5c + 20130 0. 9996 8 3 DALP 9. 23 16. 4 ~ 817 A = 517. 22c - 12798 0. 9988 10 4 DPRP 9. 44 18. 5 ~ 1107 A = 521. 11c - 7932. 5 0. 9998 10 5 DIBP 10. 25 16. 5 ~ 990 A = 1295. 4c + 6342. 5 0. 9994 10 6 DBP 11. 25 16. 6 ~ 996 A = 69467c - 5239. 5 0. 9995 10 7 DMOEP 11. 70 37. 4 ~ 747. 6 A = 51. 102c - 1033. 2 0. 9992 20 8 DMPP 12. 73 215. 4 ~ 12924 A = 1096. 5c - 351264 0. 9997 100 9 DEOEP 13. 18 80 ~ 1600 A = 22. 451c + 3622. 5 0. 9996 50 10 DAP 13. 60 66. 2 ~ 1986 A = 454. 02c - 37874 0. 9994 30 11 DHXP 16. 33 35 ~ 700 A = 120. 6c - 3081. 2 0. 9967 20 12 BBP 16. 45 35. 8 ~ 715. 4 A = 230. 15c - 3867. 2 0. 9998 20 13 DBOEP 18. 34 69. 2 ~ 1384. 6 A = 32. 269c - 854. 94 0. 9999 35 14 DCHP 19. 14 35. 3 ~ 706. 2 A = 448. 96c - 5255. 6 0. 9996 20 15 DHP 19. 49 34. 4 ~ 687. 6 A = 17. 986c - 277. 77 0. 9997 20 16 DEHP 19. 67 33. 9 ~ 677 A = 654. 74c + 12903 0. 9997 20 17 DNOP 24. 02 35 ~ 699. 2 A = 53. 06c + 668. 16 0. 9982 20 18 DINP 24. 20 ~ 28. 10 361. 5 ~ 7230. 8 A = 24. 179c - 8439. 9 0. 9990 200 19 DIDP 28. 50 ~ 31. 20 335. 4 ~ 6707. 6 A = 36. 939c + 613. 51 0. 9998 200 20 DNP 29. 40 8. 5 ~ 169. 2 A = 56. 184c + 287. 35 0. 9999 7 4 /mg kg - 1 1 2 3 4 5 6 7 8 9 /% RSD DMP 47 49 42 53 38 51 35 45 41 45 13. 33 DEP 34 28 37 36 30 38 29 32 40 34 12. 64 DIBP 38 45 33 35 47 43 41 32 36 39 13. 85 DBP 83 73 76 88 84 90 79 86 93 84 7. 86 DEHP 2145 2118 2026 2335 2264 2071 2293 1997 1959 2134 6. 37 2. 4 9 4 4 8 3 9 5 5 83. 6% ~ 104. 1% 2. 5 2 8 2013 32 3 27
5 /μg L - 1 /% /μg L - 1 /% /μg L - 1 /% 1 DMP 156. 0 104. 1 62. 4 95. 4 31. 2 92. 2 2 DEP 136. 5 95. 3 54. 6 92. 5 27. 3 91. 8 3 DALP 817. 5 94. 3 327. 0 90. 9 163. 5 93. 2 4 DPRP 184. 5 92. 7 73. 8 91. 4 36. 9 90. 8 5 DIBP 165. 0 89. 6 66. 0 92. 3 33. 0 86. 5 6 DBP 166. 0 93. 9 66. 4 94. 6 33. 2 92. 7 7 DMOEP 1869. 0 90. 3 747. 6 91. 2 373. 8 86. 7 8 DMPP 2154. 0 91. 8 861. 6 92. 5 430. 8 90. 3 9 DEOEP 4000. 0 92. 1 1600. 0 91. 5 800. 0 90. 4 10 DAP 331. 0 95. 3 132. 4 96. 1 66. 2 92. 8 11 DHXP 1750. 0 90. 5 700. 0 91. 2 350. 0 88. 7 12 BBP 1788. 5 93. 2 715. 4 92. 6 357. 7 91. 8 13 DBOEP 3461. 5 89. 8 1384. 6 90. 2 692. 3 87. 3 14 DCHP 1765. 5 89. 6 706. 2 88. 5 353. 1 85. 4 15 DHP 1719. 0 90. 6 687. 6 90. 8 343. 8 88. 4 16 DEHP 1692. 5 92. 9 677. 0 93. 1 338. 5 90. 8 17 DNOP 1748. 0 89. 8 699. 2 90. 2 349. 6 89. 4 18 DINP 18077. 0 88. 2 7230. 8 86. 7 3615. 4 83. 6 19 DIDP 16769. 0 88. 5 6707. 6 87. 4 3353. 8 85. 9 20 DNP 423. 0 90. 3 169. 2 89. 7 84. 6 86. 4 8 6 6 8 mg /kg 1 QIAN Lu-sheng CAO Li-yun LING Yong-long et al. Technical Manual for Coated Paper M. Beijing China Light Industry DMP DEP DIBP DBP DEOEP DEHP DNOP Press 2000.. M. 1 # 47 34 38 83-2145 - 2000. 2 # 185 1377 84 72 4565 2128 12 3 # - - 214 423 2061 729-2 CAO Zhen-lei. The Satuation of China Pulp and Paper Industry J. 4 # 79 - - 537-1869 93 China Pulp & Paper 2009 28 10 63. 5 # - - - 296-145 -. J. 2009 28 6 # - - - - - 638-10 63. 7 # 100 16 62 83 1276 - - 3 YIN Zhan-he JIANG Jian-fang. Application of Starch in Coated Ivory 8 # - 61 123 138-2418 - Board J. China Pulp & Paper 2009 28 7 46.. J. 2009 28 7 46. 2 4 LIU Cheng-liang LIU Chun-jing WANG Jing. Control Technology DEHP in the Process of ASA Glueing J. China Pulp & Paper 2008 27 DMP DEP DIBP DBP 2145 47 8 77. 34 38 83 mg /kg. ASA J. 3 2008 27 8 77. 5 WANG Jin LIU Cheng-liang GUO Yong-wei et al. Performance of Alkenyl Succinic Anhydride and Its Application J. China Pulp & - Paper 2010 29 1 31. GC-MS. ASA J. 2010 29 1 31. 6 HUANG Yong-hui. Simultaneous determination of 22 phthalate ester 28 China Pulp & Paper Vol. 32 No. 3 2013
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