8 6 Vol. 8 No. 6 2017 6 Journal of Food Safety and Quality Jun., 2017 X 耿志旺, 乐 * 健, 杨永健 (, 201203) 摘要 : 目的 X 方法, 80 s, 905~1852 mg/kg,,, 结果 8, 7, 1, 结论 X 关键词 : ; ; ; X Rapid screening of sulfur fumigated star anises by field-portable X-ray fluorescence GENG Zhi-Wang, LE Jian, YANG Yong-Jian * (Shanghai Institute for Food and Drug Control, Shanghai 201203, China) ABSTRACT: Objective To establish a method of rapid screening of sulfur fumigated star anises by field-portable X-ray fluorescence (XRF). Methods The sulfur content of dried fresh star anises was detected by soil model. The test time was 80 s and the result of sulfur content was 905~1852 mg/kg. Setting the sulfur content of dried fresh star anises as the reference value, the dry star anises of market were quickly screened. The samples were also tested according to the method of the Ministry of Agriculture. Results The content sulfur of 7 batches were more than standard, which should be determined as sulfur fumigated star anises, and the other one sample was not fumigated, of which the content was low than standard. The results of XRF were in accordance with the method of the Ministry of Agriculture. Conclusion The portable XRF can be used for rapid screening of sulfur fumigated star anises. KEY WORDS: star anise; sulfur fumigated; field-portable; X-ray fluorescence 1 引言,,, [1], [2],, [3] (SO 2 ),, SO 2-3, [4], - [5],,, [6],, * 通讯作者 :,,, E-mail: yongjianyang@163.com *Corresponding author: YANG Yong-Jian, Chief Pharmacist, Shanghai Institute for Food and Drug Control, Shanghai 201203, China. E-mail: yongjianyang@163.com
2278 8 X X, [7] X [8] [9] [9] [11,12] Niton XL3t 700s X [13] X,,, X,, 1,, 2 材料和方法 2.1 材料与仪器 Niton XL3t 700s X ( Thermofisher Scientific ) 5 ; 8 2.2 试验方法 2.2.1 样品前处理 5 X1 X2 X3 X4 X5; 5 105 48, G1 G2 G3 G4 G5; 8 S1 S2 S3 S4 S5 S6 S7 S8 2.2.2 测定模式的选择 X X1,, 5, 80 s 2.3 样品测定,, 5, 80 s 2.4 蒸馏 - 滴定法测定 SO 2 含量 NY/T1435-2007 [14] 8 SO 2 3 结果与分析 3.1 测试模式的选定 X,,,, - [15],,,, X1 1,, 1,,, 3.2 测定结果, 2 2, 0~567 mg/kg, 905~1852 mg/kg,,, 2, 905~1852 mg/kg, 8 7 905~1852 mg/kg, 8, 表 1 样品 X1 的土壤模式和固体模式的硫测定结果 Table 1 Result of X1 by soil and solid models 1 2 3 4 5 590 589 563 553 567 572 2.87% 431 486 403 440 453 443 6.87%
6, : X 2279 1 X Fig. 1 X-ray fluorescence spectra of fresh star anises by soil and solid models : a: (soil)b.: (solid)1. (peak of sulfur) 2 X Fig. 2 X-ray fluorescence spectra of dry star anises of market, dried fresh star anises, and fresh star anises : a: ; b: ; c: ; 1. (peak of sulfur) Table 2 表 2 新鲜八角 干燥后新鲜八角 市售干八角的硫测定值 (n=5) Apparent sulfur content of fresh, dried fresh and dry on market star anises (n=5) 1 2 3 4 5 平均 X1 567 502 487 548 516 524 X2 430 452 508 468 465 465 (mg/kg) X3 220 0 0 0 125 69 X4 0 0 0 0 0 0 X5 0 0 0 0 0 0 G1 1401 1367 1431 1399 1352 1390 G2 1232 1460 1315 1213 1297 1303 (mg/kg) G3 905 995 1054 1042 970 993 G4 1045 1120 1271 1374 1693 1301 G5 1742 1852 1765 1627 1725 1742
2280 8 续表 2 1 2 3 4 5 平均 S1 32100 30700 31200 31800 30200 31200 S2 38200 37500 36400 38600 36900 37520 S3 33300 32800 32500 33800 31900 32860 (mg/kg) S4 38300 37600 37200 36800 36400 37260 S5 28100 27500 26900 28700 29300 28100 S6 35200 34900 35600 34800 36200 35340 S7 18700 17900 17500 19300 18300 18340 S8 1252 1387 1260 1365 1305 1314 3.3 蒸馏 - 滴定法结果 - 8 SO 2 3 GB/T 7652-2006 [16] SO 2 <30 mg/kg, 7, 8, X, SO 2 X,, 表 3 市售干八角的 SO 2 含量 Table 3 Sulfur dioxide residue of dry star anises on market (mg/kg) S1 465 S2 457 S3 481 S4 490 S5 433 S6 441 S7 387 S8 6 4 结论 Niton XL3t 700s X,, 0~567 mg/kg, 8, 7, 1,,,, 参考文献 [1],,,. [J]., 2005, (5): 18 22. Wang Q, Jiang L, Wen QB. Advances in studies on Iilicium Verm [J]. Chin Condiment, 2005, (5): 18 22 [2],. [J].. 2007, (3): 5 7. Li W, Cao Y. The progress in research on star anise (IIlicium Verum Hook. F) and its extract shikimic aci [J]. Jiangsu Condiment Subsidiary Food, 2007, (3): 5 7 [3],,. [J]., 2001, 32(20): 30 35. Li J, Yang H, Li CC. Simultaneous extraction of volatile oil and shkimic acid from star anise [J]. Food Sci, 2001, 32(20): 30 35. [4],,,. GC-MS [J]., 2010, 20(8): 23 24. Liang Y, Tao Y, Zhang XH, et al. GC-MS analysis of essential oil from Illicium Verum Hook. F and its sulfur-smoke dried sample [J]. Pharm Today, 2010, 20(8): 23 24 [5],,,. [J].. 2014, 26(5): 486 488. Liao YH, Liu H, Chen K, et al. Analysis of sulfur dioxide residues in star anise in Guangxi and discussion on hygienic standard [J]. Chin J Food Hyg, 2014, 26(5): 486 488. [6],,,. [J].. 2013, 41(7): 1050 1056. Luo LP, Wang J, Zhang WJ, et al. Rapid screening of sulfur fumigated Chinese star anises by surface desorption atmospheric pressure chemical ionization mass spectrometry [J]. Chin J Anal Chem, 2013, 41(7): 1050 1056.
6, : X 2281 [7],,,. X [J]., 2012, 32(7): 1 4. Yin LH, Li JQ, Yu H, et al. The rapid detection of Cr in gelatin by X-ray fluorescence elemental analysis technology [J]. Chin J Pharm Anal, 2012, 32(7): 1 4. [8] Annie B, Murray TB, Andrew T. Novel use of field- portable-xrf for the direct analysis of trace [J]. Environ Pollut, 2016, 49(9): 1 6. [9] Alexia A, Alfred L, Roland P. Monitoring of WEEE plastics in regards to brominated flame tetardants using handheld XRF [J]. Waste Manag, 2015, 36: 297 304. [10] Ellery F. Can I get chips with that? Sourcing small obsidian artifacts down to microdebitage scales with scale with portable XRF [J]. J Archaeol Sci, 2016, 9: 448 467. [11],,,. X [J]. 2012, 32(6): 920 924. Yin LH, Li JQ, Yu H, et al. Rapid screening of Cr in vacant capsule by X-ray fluorescence elemental analysis technology [J]. Chin J Pharm Anal, 2012, 32(6): 920 924. [12],,. X [J]., 2007, 27(9): 1866 1868. Wang WJ, Guan Y, Zhu YY. Novel identification of donkeyhide glue by X-ray fluorescence analysis [J]. Spectrosc Spect Anal, 2007, 27(9): 1866 1868. [13],,,. X [J]., 2006, 13(1): 13 15. Jian H, Wu SP, Yao GS, et al. The method of energy-dispersive X-ray fluorescence spectrometer and its application [J]. Electr Qual, 2006, 13(1): 13 15. [14] NY/T 1435-2007 [S]. NY/T 1435-2007 Determination of total sulphr dioxide content-fruit, vegetable, and derived products [S]. [15],,,. X [M]. :, 2001. Ji A, Tao GY, Zhuo SJ, et al. X-ray flurosescence spectrum analysis [M]. Beijing: Science Press, 2001. [16] GB/T 7652-2006 [S]. : GB/T 7652-2006 Star anises [S]. 作者简介 ( 责任编辑 : 姜姗 ) 耿志旺, 硕士, 主要研究方向为药物分析 快检方法 E-mail: gengzhiwang@sina.com 杨永健, 博士, 硕士生导师, 主要研究方向为药品质量标准 快检方法 E-mail: yongjianyang@163.com