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43 208 no_pw
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Q Q Vol. 43, No. 4 Q QQ Q Q QQ Q Q Q 14 2Q4 Q , Q QQ QQ QQ Q Q Q Determination of Organotin Compounds in Plastic Products by GC/MS after Ethyl Derivatization with Sodium Tetraethylborate Hiroyuki O=CD , Masako SJOJ@>, Shigehito N6@6H=>B6, Taiki ADN6B6 and Kazunori M>I6C> (Nagoya City Public Health Research Institute: 1 11, Hagiyama-cho, Mizuho-ku, Nagoya 467 8615, Japan; Corresponding author) A simultaneous determination method for 9 organotin compounds in polyvinyl chloride (PVC) and silicone products used as kitchen utensils and food packages was developed using ethyl derivatization with sodium tetraethylborate (NaBEt4). Organotin compounds were extracted with acetone hexane (3 : 7) from the samples after acidification and the extract was filtered and concentrated at under 40 . After centrifugal separation, these compounds were derivatized with 2 NaBEt4 solution and determined by GC/MS. This method was applicable for simple routine analysis. Recoveries of spiked compounds were 49.1 118.1 for 3 PVC products and 88.8 102.2 for a siliconized paper. Monooctyltin, dioctyltin and trioctyltin compounds were found in all PVC food containers at the levels of 123 1,380 mg/g, 1,770 13,200 mg/g and 6.6 139 mg/g, respectively. They also were found in 3 gloves, 5 spouts, 1 hose and 5 pipes. Some PVC products contained monomethyltin, dimethyltin, trimethyltin, monobutyltin and dibutyltin compounds at the levels of 97.3 433 mg/g, 96.5 5,120 mg/g, 8.5 24.9 mg/g, 1.2 852 mg/g and 1.2 29.4 mg/g, respectively. (Received February 4, 2002) Key words: Q QQ organotin compounds; Q plastic products; Q polyvinyl chloride; Q QQ Q Q kitchen utensils and food packages; QQ ethyl derivatization; Q sodium tetraethylborate; /Q Q GC/MS QQ Q Q Q Q Q Q Q QQ Q (PVC) Q QQQ Q Q 1) QQ QQQ Q QQ Q Q Q Q PVC Q Q Q Q Q Q 2) 1 1.5 QQ Q Q Q QQ 3) 4) 5) 6) Q QQ QQ Q Forsyth QQ QQ Q Q QQ Q Q Q Q Q QQQ QQ Q QQ Q 50 mg/g Q QQ Q QQ Q Q Q QQ Q Q Q Q Q QQQ Q Q Q Q QQQ Q QQ Q Q Q Q Q QQ QQ Q Q QQ Q Q Q Q Q QQ Q QQ Q Q Q 2), 5) QQQ QQQQ 467 8615 QQQQ Q Q GC-FPD Q 2) 1 11 QQ Q QQ Q
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August 2002
QQ Q Q Q QQ QQQ Q Q 209 QQQ Q QQ QQ GC-ASS4), GC/MS5) Q 1 mL Q Q Q 100 mL (10 6) Q QQQ Q Q Q mg/mL) QQ Q2), 4) 6) Q Q Q QQ Q QQ Q Q QQQ QQ QQ QQQ Q Q Q Q QQ Q Q Q Q Q Q Q Q Q Q NaBEt4 QQ NaBEt4 Strem Chemicals 0.4 g Q Q Q Q Q (NaBEt4) Q 20 mL Q 2 QQ Q QQ Q7) 9) QQ Q QQ NaBEt4 QQ QQ Q Q Q QQ Q (pH 5.0): 2 mol/L Q Q Q Q QQ 2 mol/L Q Q 5.9 : 14.1 QQ QQ QQQ 9 Q GC/MS Q Q QQ Q QQQ QQ Q QQ QQQQ Q Polyvinyl chloride n PVC QQ Q Q Q 80 Q QQQ 1,100 QQ QQQ Q Q QQ 3. GC / MS Hewlett Packard HP 6890 Q GC HP5973 QQ Q Q 1. Q Q Whatman GF/B (5.5 cm) QQQ Q QQ QQ QQ 80 Q Q 20 mL 4. 1) PVC Q 54 Q 1) Q QQQ QQ 22 Q QQ Q QQ Q Q Q Q Q 0.5 g Q QQ QQQ QQ QQ QQQ Q Q (3 : 7) QQ 20 mL Q QQ 1 Q 8Q Q QQ QQQQ Q6Q Q Q 37 QQ QQ Q Q QQ 3Q Q Q 6Q Q QQ Q Q Q Q Q QQQ Q Q QQQ QQ Q Q Q Q Q QQQ Q 20 30 mL Q QQ 2 Q Q QQ 4 Q Q Q Q Q Q Q Q Q Q Q5Q QQ QQQ Q Q Q Q 1 mL QQQ 40 QQ Q Q Q Q Q Q Q Q Q 20 mL 2) Q Q Q 26 Q Q Q QQ Q 840 10 Q Q Q Q QQQ Q 8Q Q Q QQQ QQ QQQ QQ QQ 3Q Q Q Q Q Q QQ Q Q Q Q 1Q Q3Q QQQ Q 3Q 2) QQ Q QQQQQ Q QQ Q 6Q QQQQ Q Q QQ Q (pH 5.0) 5 mL QQQ Q2Q Q Q Q 0.25 mL Q Q QQ QQQ 2 mL Q 2. 2 NaBEt4 1 mL Q Q 20 QQQ QQ Q QQ Q QQ Q Q Q (MMT) Q Q Q Q Q1 Q Q Q (MBT) Q Q (DMT) QQ 3) GC/MS Q (TMT) QQQQ Aldrich Q Q 1 mL Table 1 GC/MS Q (DBT) Q Q Q (TBT) QQQ QQ QQQ Q Q QQQ Q QQ Q Q (DOT) QQQ Lancas- QQ QQQ QQ ter Q Q (TOT) QQQ Fluka QQ Q Q (3 : 7) QQ 20 mL QQ Chemie Q Q 40 mg Q 20 mL Q QQQ Q Q Q Q Q Q Q Q Q Q QQ (2,000 mg/mL) Q Q Q Q Q QQQ Q QQ (MOT) QQQ Q Q Q Q Q 10) QQ QQQ Q 31.3 mg QQ 15 mL Q QQ 1 Q QQ Q Q 20 mL ( QQQ 2,000 mg/mL) 1. 6) QQ QQQ Q QQ QQ Q Q Q Q QQ QQQ QQ Q QQ 2 100 mg/mL Q Q (3 : 7) QQ QQQ QQ Q QQQ Q Q Q (TeBT) Merck QQ QQ QQ QQ 100 mg Q QQ 100 mL Q Q Q Q QQQQ QQ Q
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Q Vol. 43, No. 4 Table 1. GC/MS Conditions for Determination of Orga- Q Q QQ QQQ Q QQ notin Compounds Q GC/MS Q Q Q Column : HP-5 ms (30 m 0.25 mm i.d., QQ QQ Q 0.25 mm film thickness) QQ QQ Carrier gas : He, 10.0 kPa Temperature 2. Oven : 45 (4 min) 15 /min 300 (4 min) NaBEt4 Q Q Q Q Q Injector : 290 Q pH, NaBEt4 QQQ Q Q QQ Interface : 300 Ion source : 230 Q pH 3.6 5.6 Q Q 100 mg/g Injection method : splitless, purge o# 1 min QQQ 2 mL Q 0.2 2 mL 2 NaBEt4 Injection volume : 1 mL Q Q 5 60 QQQ Ionization method : EI Ions measured for quantitation: QQQ GC/MS Q Q pH Q MMT: 193 (191, 189), DMT: 179 (177, 175), Q pH 4.0 QQ TMT: 165 (163, 161), MBT: 235 (233, 231), pH 4.6 5.6 Q pH 5.0 DBT: 263 (261, 259), TBT: 291 (289, 263), MOT: 291 (289, 287), DOT: 375 (373, 371), NaBEt4 QQ 0.2 mL TOT Q TOT: 375 (373, 459), TeBT: 291 (289, 287) QQ 0.5 mL Q Mass numbers in the parentheses are ions used for Q QQ Q Q 10 QQ confirmation. QQQ Q Q QQ Q Q Q Q QQQ Q Q QQ QQ 2 NaBEt4 QQ 1 mL Q Q 20 Q Q Q Q Q 5 Q Q QQ QQQ Q QQ 3. GC/MS Fig. 2 9 Q Q TeBT QQ QQ Q QQQ QQ Q QQQQQ 1.0 mg/g QQ Fig. 1. Extraction e$ciency for MOT from 8 kinds of samples Q Q Q Q 1st extract; 2nd extract; 3rd extract QQ QQ Q QQ 1.0 500 mg/g Q Q QQ QQ 0.9981 QQQ Q Q Q Q Q 0.9999 Q Q Q Q QQ 3 QQ Q Q Q Q QQQ QQ Q Q Q Q Q Q Q QQ Q Q Q QQQQ DOT Q Q QQQQ Q Q Q No. 13 Q Q Q QQ QQQ Q No. 7 Q No. 16, GC/MS Q (Table 1) Q Q DBT Q Q No. 3 Q No. 3 Q QQ QQ Q Q QQ Q Q QQQ Q Q Q QQ Q Q 2Q Q Q Q Q 3Q (No. 3, No. 4, No. 6) Q Q Q Q DBT Q Q Q MMT, DMT, DBT, DOT Q TOT 1 QQ MOT Q DOT Q Q Q Q 94 Q MBT MOT TeBT Q QQQQ No. 13 Q Q 70.8 4. 80.9 Q Q Q Q Q QQ PVC Q Q3Q Q 10 mg/g Q QQ Q Fig. 1 MOT QQ 100 mg / g QQ Q Q (Table 2) QQ Q QQ Q Q Q QQ PVC No. 1 QQQ QQQ Q Q Q Q QQQQ Q Q 83.2 107.7 Q 88.8 102.2 QQ Q Q QQ QQ Q 0.7 8.6 Q 0.5 4.0 9 QQQ Q Q QQ Q QQ Q QQ6) Q Q Q QQ Q Q Q Q QQ Q Q QQ QQ Q QQ No. 1 No. 2 MMT 49.1 Q Q Q Q QQ 63.3 MMT QQQ Q
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August 2002
QQQ QQQ Q QQ QQQ 211 Fig. 2. Typical chromatograms of organotin compounds by GC/MS after ethyl derivatization (A): Standard solution (100 mg/g as chloride of each), (B): Food container No. 7 (five times dilution), (C): Hose No. 3 (two times dilution), (D): Pipe No. 3 (two times dilution) 1: Trimethyltin (TMT), 2: Dimethyltin (DMT), 3: Monomethyltin (MMT), 4: Monobutyltin (MBT), 5: Dibutyltin (DBT), 6: Tributyltin (TBT), 7: Monooctyltin (MOT), 8: Dioctyltin (DOT), 9: Trioctyltin (TOT), IS: Tetrabutyltin (TeBT) Table 2. Recoveries of Organotin Compounds from 4 Kinds of Spiked Samples Added Recovery ( ) Sample (mg/g) MMT DMT TMT MBT DBT TBT MOT DOT TOT Polyvinyl chloride 10 90.4 8.6 107.7 2.8 94.0 2.3 90.4 4.7 96.6 1.2 99.9 0.7 95.4 5.0 100.7 3.8 95.5 1.1 (Powder) 100 83.2 4.7 102.2 2.2 105.0 3.7 85.1 2.7 99.4 0.9 101.2 1.1 88.0 3.4 97.6 1.8 95.9 3.4 Wrapping film 10 49.1 5.2 99.8 2.3 95.9 4.3 75.8 4.7 97.3 0.9 98.4 1.2 118.1 5.2 102.0 1.5 108.3 4.0 No. 1 100 51.2 3.5 94.7 2.6 96.1 2.0 82.7 3.1 96.6 1.2 100.9 1.3 115.0 4.6 98.3 5.9 101.2 2.1 10 61.7 5.7 91.1 2.8 92.3 2.8 76.6 3.8 99.0 2.9 98.3 1.9 96.7 4.3 105.5 5.2 116.3 4.2 Gloves No. 2 100 63.3 4.7 86.1 3.1 91.3 1.7 78.4 5.4 98.1 1.6 100.1 1.4 104.0 3.9 113.0 4.6 108.0 4.5 Cooking sheet 10 90.6 3.0 97.6 1.9 98.5 2.6 96.7 2.0 98.9 2.0 100.7 0.8 96.6 1.6 102.2 4.0 98.5 2.6 No. 1 100 88.8 2.4 99.5 1.7 98.9 1.1 94.3 2.1 98.5 0.5 99.7 0.7 99.1 2.3 97.9 0.6 102.0 1.8 Each value is the mean S.D. of four determinations. QQ Q QQQ Q QQQ Q Q mg/g) 1 QQ QQ QQ Q QQ Q Q Q DOT QQ Q Q 8Q QQ 75.8 QQ QQQQ Q Q MOT TOT 118.1 QQ QQ Q QQ Q Q QQ Q QQ DMT QQ 4 Q QQQQ QQ Q QQ DOT QQ QQ Q QQ Q 5. QQQQ Q Q MMT Q TMT QQ PVC QQ 54 QQQ QQQQ 26 QQ Q DOT MOT QQ Q QQ Q QQ QQ Table 3 Q No. 8 QQQ Q Table 4 QQ DBT QQ QQ 1) PVC QQQQQ QQ Q Q QQ QQ QQ 22 QQ QQ QQ MBT QQ Q DOT QQQ DOT QQ (1,770 13,200 mg/g) Q Q Q Q Q Q Q MOT (123 1,380 mg/g), TOT (6.6 139 mg/g) 2) PVC QQQ Q Q 4 QQ QQ 8 QQQ 3 QQ DOT 358 391 mg/g, QQ DMT (1,060 1,510 mg/g), MMT (118 197 MOT 40.7 113 mg/g, TOT 3.8 8.2 mg/g QQ mg/g), TMT (8.5 13.1 mg/g) Q QQ QQ No. 1 QQ No. 6 Q Q QQ DBT (1.2 10.4 mg / g) 4 QQ MBT (2.4 No. 7 QQQ QQ Q
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Vol. 43, No. 4 Table 3. Contents of Organotin Compounds in PVC Products Content ( mg/g) Sample No. Use MMT DMT TMT MBT DBT TBT MOT DOT TOT Food container 1 n.d. n.d. n.d. n.d. n.d. n.d. 602 9,280 52.9 Worcester sauce 2 n.d. n.d. n.d. n.d. n.d. n.d. 466 9,200 67.5 Worcester sauce 3 n.d. n.d. n.d. n.d. n.d. n.d. 407 8,350 51.1 Worcester sauce 4 n.d. n.d. n.d. n.d. n.d. n.d. 551 3,350 18.7 Tartar sauce 5 n.d. n.d. n.d. n.d. n.d. n.d. 705 12,700 97.1 Soy sauce 6 n.d. n.d. n.d. n.d. 1.2 n.d. 399 10,900 28.6 Laver 7 176 1,220 13.1 n.d. n.d. n.d. 506 6,560 97.9 Laver 8 n.d. n.d. n.d. 2.4 4.4 n.d. 1,380 1,900 13.9 Laver 9 n.d. n.d. n.d. n.d. 1.6 n.d. 855 11,800 79.3 Laver 10 n.d. n.d. n.d. n.d. n.d. n.d. 474 12,600 31.3 Laver 11 n.d. n.d. n.d. n.d. n.d. n.d. 498 10,000 54.2 Laver 12 n.d. n.d. n.d. n.d. n.d. n.d. 564 10,900 86.6 Pickled ume 13 n.d. n.d. n.d. n.d. n.d. n.d. 642 13,200 139 Sesame seed 14 n.d. n.d. n.d. n.d. n.d. n.d. 405 8,800 64.1 Candy 15 n.d. n.d. n.d. n.d. n.d. n.d. 388 7,710 115 Candy 16 197 1,510 10.0 n.d. n.d. n.d. 355 8,390 35.0 Rice cracker 17 133 1,110 8.5 n.d. n.d. n.d. 391 7,310 47.5 Dried squid 18 118 1,060 10.3 n.d. n.d. n.d. 394 7,260 50.0 Dried squid 19 n.d. n.d. n.d. n.d. n.d. n.d. 364 11,500 28.0 Fried fish 20 n.d. n.d. n.d. n.d. n.d. n.d. 331 4,150 34.1 Tart 21 n.d. n.d. n.d. n.d. n.d. n.d. 925 5,030 27.4 Pudding 22 n.d. n.d. n.d. n.d. 10.4 n.d. 123 1,770 6.6 Salad Gloves 1 n.d. n.d. n.d. n.d. n.d. n.d. 113 391 8.2 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Disposable 4 n.d. n.d. n.d. 1.2 4.0 n.d. n.d. n.d. n.d. 5 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 6 n.d. n.d. n.d. n.d. n.d. n.d. 40.7 358 4.6 7 n.d. n.d. n.d. n.d. n.d. n.d. 43.4 364 3.8 8 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Spout 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Teapot 2 n.d. n.d. n.d. n.d. 1.6 n.d. 953 839 25.9 Teapot 3 n.d. n.d. n.d. n.d. 22.7 n.d. 979 754 3.6 Teapot 4 n.d. n.d. n.d. n.d. n.d. n.d. 266 5,160 50.8 Teapot 5 n.d. n.d. n.d. n.d. n.d. n.d. 585 709 10.2 Earthen teapot 6 n.d. n.d. n.d. n.d. 1.6 n.d. 866 790 24.7 Teapot Hose 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Home use 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 3 97.3 560 n.d. n.d. 29.4 n.d. 54.8 1,330 n.d. Pipe 1 102 96.5 n.d. n.d. 1.7 n.d. 6.2 74.2 n.d. Water supply 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Water supply 3 n.d. n.d. n.d. 852 1.4 n.d. 131 2,320 13.0 Water supply 4 n.d. n.d. n.d. 560 1.5 n.d. 165 2,880 12.1 Water supply 5 433 5,120 24.9 n.d. 4.6 n.d. n.d. 6.0 n.d. Hot-water supply 6 n.d. n.d. n.d. n.d. n.d. n.d. 411 5,120 33.9 Hot-water supply Wrapping film 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Home use 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Home use 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Home use 4 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Home use Mat 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Luncheon mat 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Luncheon mat 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Nonskid mat 4 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Nonskid mat 5 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Sink mat Each value is the mean of two or three determinations, expressed as chloride form. n.d.: 1.0 mg/g
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QQQ QQQ Q Q QQQ 213 Table 4. Contents of Organotin Compounds in Silicone Products Content ( mg/g) Sample No. Use MMT DMT TMT MBT DBT TBT MOT DOT TOT Cooking sheet1) 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 4 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 5 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 6 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 7 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 8 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Paper cup1) 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Cooking mat2) 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 2) Cooking spatula 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Packing2) 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Food container 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Lunch box 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Lunch box Nipple2) 1 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 2 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 3 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 4 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 5 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 6 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Spout2) 7 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Teapot 8 n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. Teapot Each value is the mean of two determinations, expressed as chloride form. n.d.: 1.0 mg/g 1) Siliconized paper 2) Silicone rubber QQ Q DOT 4) PVC Q Q QQQ Q Q MOT TOT QQ 3 Q Q QQQ Q Q QQ QQ Q QQ Q No. 4 DBT (4.0 mg/g) MBT (1.2 mg/ Q QQ 3 QQ 2 Q g) Q QQ Q Q QQQ QQ No. 3 Q Q Q Q QQ Q Q Q Q DOT 1,330 mg/g, DMT 560 mg/g, MMT 97.3 mg / g, MOT 54.8 mg / g, DBT 29.4 3) PVC QQ mg/g Q DOT DMT QQ 6 QQ No. 2 No. 6 5 Q DOT Q Q QQQ Q Q 709 5,160 mg/g, MOT 266 979 mg/g, TOT MMT, MOT DBT Q 3.6 50.8 mg/g Q No. 2, No. 3, No. 6 3 Q DBT 1.6 22.7 mg/g Q No. 4 Q 5) PVC Q QQQQ QQ DOT QQ DOT 6 QQ No. 2 Q Q No. 1 No. Q Q QQQ Q Q 3 No. 6 5 Q Q Q No. 3 MOT TOT Q QQ Q 4 Q No. 4 QQ QQQQ Q Q DOT MOT QQ 500 1,000 mg/g Q DOT 2,320 2,880 mg / g, MBT 852 560 QQQ DOT MOT Q mg / g, MOT 131 165 mg / g, TOT 13.0 Q Q 12.1 mg/g, DBT 1.4 1.5 mg/g Q DOT DBT Q QQ Q QQQ MBT Q Q MOT TOT DOT QQ QQQ Q Q DBT DOT Q MBT
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Q Q Vol. 43, No. 4 QQQ Q Q QQQ Q Q QQQQQ 2 QQ QQ Q QQ Q No. 5 DMT 5,120 mg/g, MMT 433 mg/g, TMT 24.9 mg/g, DOT 1) Ohno, H., Suzuki, M., Iwama, M., Nakashima, S., Aoyama, T., Yamamoto, K., A comparison of analyti- 6.0 mg / g, DBT 4.6 mg / g Q Q QQ cal methods for dibuthyltin compounds in polyvinyl DMT Q MMT QQQ Q Q chloride products. Nagoyashi Eiseikenkyusho Ho TMT, DOT, DBT QQQ QQ No. 6 (Annual Report of Nagoya City Public Health DOT 5,120 mg / g, MOT 411 mg / g, TOT 33.9 Research Institute), 42, 17 20 (1996). mg/g QQ DOT QQ MOT QQQ 2) Takami, K., Okumura, T., Yamasaki, H., Nakamoto, M., Q Q TOT QQQ Q Determination of organotin compounds in polyvinyl chloride products by GC. Bunseki Kagaku, 37, 117 QQ QQ No. 1 MMT, DMT, DOT, 122 (1988). MOT DBT QQ Q QQ Q 3) Nakashima, H., Hori, S., Nakazawa, H., Determination QQ Q Q (1.7 102 mg/g) of dibutyltin and dioctyltin compounds in PVC food 6) PVC Q containers, wrappage and clothes by reversed phase QQ Q 4 QQ QQ Q HPLC with column switching. Eisei Kagaku, 36, 15 20 5 QQ QQ (1990). 4) Forsyth, D. S., Dabeka, R., Sun, W. F., Dalglish, K., Speci- QQ QQ ation of organotins in poly(vinyl chloride) products. 7) QQQQ Food Addit. Contam., 10, 531 540 (1993). QQQ 8 QQ 5) Takahashi, S., Mukai, H., Tanabe, S., Sakayama, K., 3 QQ Q Miyazaki, T., Masuno, H., Butyltin residues in livers of 1 QQ 3 QQ 3 QQ humans and wild terrestrial mammals and in plastic QQ 6 QQ Q Q 2 QQ QQ 26 QQ QQ products. Environ. Pollut., 106, 213 218 (1999). 6) Kawamura, Y., Maehara, T., Suzuki, T., Yamada, T., QQ QQ 5), 6) Determination of organotin compounds in kitchen DBT QQ QQ utensils, food packages and toys by gas chromatogra- Q QQ QQ phy/atomic emission detection method. Shokuhin Eiseigaku Zasshi (J. Food Hyg. Soc. Japan), 41, 246 253 (2000). QQ QQQ QQ 9 Q 7) Ashby, J. R., Craig, P. J., Speciation for analysis of organotin compounds by GC AA and GC MS after QQQQ NaBEt4 Q GC/MS ethylation by sodium tetraethylborate. Appl. Organo- (SIM) QQ Q Q QQ Q Q met. Chem., 5, 173 181 (1991). Q Q QQ Q Q QQ Q 8) Kuballa, J., Wilken, R., Jantzen, E., Kwan, K. K., Chau, Q Q Q Q QQ Y. K., Speciation and genotoxicity of butyltin com- QQ Q QQ QQ Q 80 QQ QQ pounds. Analyst, 120, 667 673 (1995). Q DOT PVC Q QQ 22 QQ QQ 3 9) Iwamura, T., Kadokami, K., Jin-ya, D., Tanada, K., Deter- mination of organotin compounds in biological sam- QQ Q Q 5 QQ 1 QQ 3 QQ ples using ethyl derivatization and GC / MS. Bunseki DMT QQ 4 QQ 1 QQ Kagaku, 49, 523 528 (2000). 1 QQ MBT 2 QQ QQ 10) Hasegawa, K., Utsunomiya, A., Setsuda, S., Determina- mg/g QQQ QQ QQ Q tion of organotin compounds in textile products QQ Q MMT, TMT, DBT, MOT by gas chromatography/mass spectrometry. Kana- TOT QQ QQ Q QQ mg/g QQ gawaken Eiseikenkyusho Kenkyuhokoku (Bulletin of Kanagawa Prefectural Public Health Laboratory), 24, QQ QQQQ Q Q QQQQ QQQ Q 38 42 (1994). Q Q Q QQ Q Q QQ QQ Q Q
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