394 1 2 1 1 3 4 5 1 1 1 1. 510300 2. 510275 3. 526060 4. 526060 5. 517000 4-283. 3 nm - 2. 2% 1. 8 ~ 40. 0 μg /L 0. 5 g 10 ml 0. 036 mg /kg R155. 5 P618. 42 DOI 10. 13590 /j. cjfh. 2015. 04. 010 A 1004-8456 2015 04-0394-05 The determination of lead and interference elimination in high salty food by GFAAS HU Shu-guang SU Zu-jian CAI Wen-hua HE Jian-fei OU Tian-cheng HUANG Zhen-bo HUANG Wei-xiong LIANG Xu-xia ZHANG Xue-wu Reference Laboratory of Heavy Metals of National Food Safety Risk Monitoring Guangdong Provincial Centre for Disease Control and Prevention Guangdong Guangzhou 510300 China Abstract Objective A method of determination of lead in high salty food by GFAAS was established and the interference model various matrix modifiers temperature program and correction model were explored. Methods Lead in high salty food was measured by standard addition method with Pd NO 3 2 -NH 4 H 2 PO 4 as mixed matrix modifier after four kinds of pretreatment methods including microwave digestion wet digestion high-pressure tank digestion and direct dilution were adopted. Results While the salinity was below 2. 2% the interference could be eliminated by standard addition method with Pd NO 3 2 -NH 4 H 2 PO 4 at the wavelength of 283. 3 nm. The linear range was 1. 8-40 μg /L. When 0. 5 g sample were diluted to 10 ml the limit of quantification was 0. 036 mg /kg.conclusion This method could eliminate the interference of high salinity during lead determination by GFAAS and improve the accuracy and reliability. The study provided good technical reserves for the revision and integration of national standards were established. Key words High-salt foods lead graphite furnace atomic absorption spectrometry trace analysis food contaminant food safety 1 2-3 4 2010 5-6 JECFA 7 8 9 2015-02-13 A2013068 2014 ZHENGHE-2014-347 E-mail tony_hsg@ 163. com 1. 0 mg /kg 2 mg /kg
395 2 ~ 3 1 1. 1 VARIAN-240Z 0. 001 g 10 ml Varian MWS-2 Milestone ETHOS A 1. 2. 2 AED-440 LabTech-EH20B 283. 3 nm - 0. 2 0. 5 nm 8 ~ 12 ma 85 ~ 130 + 20 g /L GSB G 62071-90 8201 1 000 mg /L 4 ~ 5 s 100 μg /L 1. 2 1. 2. 1 0. 2 ~ 0. 6 g 0. 001 g 5 ml 5 μl 25 ~ 140 10 min 140 ~ 160 10 min 160 ~ 190 20 min 140 ~ 160 0. 5 ~ 1. 0 ml 100 μg /L 0 0. 50 1. 00 10 ml 2 ~ 1. 50 2. 00 3. 00 ml 0. 5 ~ 3 g 0. 001 g 10 ml 0. 5 ml 120 0. 5 ~ 1 h 180 2 ~ 4 h 200 ~ 220 2 10 ml 2. 1 0. 3 ~1 g 0. 001 g 5 ml 217. 0 283. 3 nm 140 ~ 160 4 ~ 5 h 217. 0 nm 140 ~ 160 283. 3 nm 0. 5 ~ 1. 0 ml 10 ml 0. 5 ~ 2 g 30 ~ 50 s 600 ~ 800 20 s 2 000 ~ 2 300 1. 2. 3 1 99 V /V 6 0 ~ 30. 0 μg /L 10 μl - 0. 2 + 20 g /L 1. 2. 4 1. 00 ml 10 ml 3 10 μl - /nm Table 1 1 5 μl 10 1 283. 3 nm Parameters of lead determination in saline solution between two sensitive lines LOD LOQ RSD RSD 0. 1% NaCl RSD 0. 5% NaCl 217. 0 0. 997 2 0. 60 2. 0 3 7 10 283. 3 0. 999 9 0. 43 1. 4 2 2 3 RSD 20 μg /L 7 LOD LOQ 21 2. 2-1 20 μg /L 283. 3 nm 450 550 650 450 550 650 3
396 11 501 950 450 550 650 11-12 283. 3 nm 450 0. 8% 550 650 1. 4% 1. 6% 2 Figure 2 - Ash temperature-absorbency curves of different matrix modifiers Figure 1 1 3 - Salinity-recover curves of three ash temperatures Figure 3 Atomic temperature-absorbency curves of different 2. 3 matrix modifiers 2. 3. 1-1% 1% 1% 650 1 800 1% 7 13 2. 3. 2 3 20 μg /L - 1 800 4 20 μg /L 600 500-2 2 500 20 μg /L - 450-3 2 650 2 - Table 2 Best temperature programming of different matrix modifiers / / 450 1 200 0. 166 2 0. 8 20 g /L 500 1 350 0. 159 4 1. 0 20 g /L 500 1 250 0. 121 2 1. 2 0. 2 g /L 600 1 600 0. 205 7 1. 4-20 + 0. 2 g /L 650 1 800 0. 219 4 1. 6 GB 5009. 12 2010 7 3-11 14-15 - 1. 6% - 1. 6% > 1. 4% > 1. 2% > 1. 0% > 0. 8%
397-0% ~ 2. 2% - Figure 4 4 - Salinity-recover curves of different matrix modifiers 2. 3. 3 2 3 4 5-2 Figure 5 Salinity-recover curves between two calibration modes - 3 2. 4-20 μg /L - 2. 5 4 5 4 4 4 0% ~ 1. 6% Table 3 3 Parameters of lead determination between two calibration modes LOD LOQ r / mg /kg 2. 0 ~ 40. 0 y = 0. 00821x - 0. 00047 0. 999 6 0. 6 2. 0 0. 040 1. 6 1. 8 ~ 30. 0 y = 0. 00320x + 0. 00857 0. 998 9 0. 5 1. 8 0. 036 2. 2 0. 5 g 10 ml / mg /kg 4 4 Table 4 Recovers and precisions of lead determination of four digestions n = 7 / mg /kg n = 3 / mg /kg n = 7 / mg /kg n = 3 / mg /kg 0. 100 0. 318 106 0. 182 98 0. 200 0. 202 2. 1 0. 402 99 0. 081 2. 4 0. 292 95 0. 400 0. 591 92 0. 460 104 0. 100 0. 296 90 0. 190 101 0. 200 0. 193 4. 5 0. 397 104 0. 079 3. 0 0. 304 109 0. 400 0. 593 92 0. 462 95 0. 100 0. 306 90 0. 183 103 0. 200 0. 400 0. 203 2. 5 0. 404 0. 590 106 96 0. 080 2. 3 0. 284 0. 473 102 95 0. 100 0. 306 98 0. 180 101 0. 200 0. 204 1. 5 0. 404 98 0. 080 1. 0 0. 281 99 0. 400 0. 601 104 0. 484 102
398 2. 6 5 < 0. 036 ~ 0. 77 mg /kg Biometals 4 Heard M J Chamberlain A C. Effect of minerals and food on uptake of lead from the gastrointestinal tract in humans J 5 mg/kg Human Toxicology 1982 1 4 411-415. Table 5 Lead content in some high salty food in Guangdong 5. J. 2009 21 2 172-182. 16 0. 14 0. 19 < 0. 036 ~ 0. 27 6 Smith M. Food safety in Europe FOSIE risk assessment of 17 0. 05 < 0. 036 < 0. 036 ~ 0. 17 chemicals in food and diet overall introduction J. Food and 15 0. 05 < 0. 036 < 0. 036 ~ 0. 10 Chemical Toxicology 2002 40 2 /3 141-144. 12 0. 10 0. 08 < 0. 036 ~ 0. 18 7. GB 5009. 12 2010 24 0. 08 0. 04 < 0. 036 ~ 0. 30 15 0. 07 0. 05 < 0. 036 ~ 0. 22 S. 2010. 17 0. 12 0. 17 < 0. 036 ~ 0. 77 8. 21 0. 06 0. 08 < 0. 036 ~ 0. 16 J. 2012 28 2 187-189. 22 0. 04 < 0. 036 < 0. 036 ~ 0. 08 3 1 Reily C. M.. 15. 1986 90-130. 2 Eklund G Oskarsson A. Exposure of cadmium from infant formulas and weaning foods J. Food Additives and Contaminants 1999 16 12 509-519. 3 Oskarsson A Widell A Ing-Marie O et al. Cadmium in food chain and health effects in sensitive population groups J. 2004 17 5 531-534. 9. GB 2762 2012 S. 2013. 10. - J. 2006 15 4 66-67. 11. GFAAS J. 2011 8 138-142 12. - J. 2013 30 6 3017-3021. 13. J. 2003 39 7 430-433. 14. GFAAS J. 2008 18 4 626-627. J. 2008 27 477-480. 7 22 Novaluron 2015 7 22 / ppm Novaluron Avocado 0. 6 Bean succulent 0. 7 Carrot 0. 05 12 ~ 12A Cherry subgroup 12-12A 8 11 ~ 10 Fruit pome group 11-10 3 12 ~ 12B Peach subgroup 12-12B 1. 9 Plum prune dried 3 12 ~ 12C Plum subgroup 12-12C 1. 9 9 Vegetable cucurbit group 9 0. 2 8 ~ 10 http / /news. foodmate. net /2015 /07 /320697. html Vegetable fruiting group 8-10 1