Microsoft Word 刘印平-二校出3836-

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1 6 10 Vol. 6 No Journal of Food Safety and Quality Oct., 2015 N,N- 刘印平 1, 刘玉欣 1, 云鹏 1, 路杨 1, 王丽英 1, 常凤启 1, 杨立新 (1.,, ; 2., ) 1, 2* 摘要 : 目的 - (gas chromatography-mass spectrometry, GC-MS) N,N- 方法, SILICA/PSA /, D6-N,N- 结果 66.9%~103.4%, (RSD) 2.5%~7.7%, 30 N,N-, 8 2, N,N- 3.0 µg/kg 结论,, N,N- 关键词 : N,N- ; - ; ; ; Determination of N-dimethyl nitrosamine in beer and sausage LIU Yin-Ping 1, YUN Peng 1, LU Yang 1, WANG Li-Ying 1 1, 2*, YANG Li-Xin (1. Hebei Provincial Center for Disease Control and Prevention, Hebei Provincial Key Laboratory of Food Safety Risk Monitoring, Shijiazhuang , China; 2. College of Environmental Sciences and Engineering, Peking University, Beijing , China) ABSTRACT: Objective To establish a method for the determination of N-dimethyl nitrosamine in beer and sausage by gas chromatography-mass spectrometry. Methods Homogenized samples sequentially were extracted by methylene chloride, centrifugation, and SILICA/PSA columns cleanup before analyzed by gas chromatography-mass spectrometry. Quantification of N-dimethyl nitrosamine was based on the use of D6-N-dimethyl nitrosamine. Results The present method showed acceptable recoveries of 66.9%~103.4%, with relative standard deviation (RSD) ranging from 2.5% to 7.7%. Analysis of 30 beer samples and 8 sausage samples by the current method were successfully performed. N,N-dimethyl nitrosamine were not detected in beer samples. Two positive sausage samples were detected and the content was lower than the limited value of 3.0 µg/kg in meat products. Conclusion This quantitative method is demonstrated to be rapid, simple, and high sensitive, which can be applied in the accurate determination of N-dimethyl nitrosamine in beer and sausage. KEY WORDS: N-dimethyl nitrosamine; gas chromatography-mass spectrometry; internal standard; beer; sausage * 通讯作者 :,, yanglixin241@163.com *Corresponding author: YANG Lin-Xin, Senior Technical Personnel, Hebei Provincial Center for Disease Control and Prevention, No.97, Huai an East Road, Shijiazhuang , China. yanglixin241@163.com

0 µg/kg 结论,, N,N- 关键词 : N,N- ; - ; ; ; Determination of N-dimethyl nitrosamine in beer and sausage LIU Yin-Ping 1, YUN Peng 1, LU Yang 1, WANG Li-Ying 1 1, 2*, YANG Li-Xin (1.

2 10, : N,N 引言 N,N- (NDMA), N-,,, [1-3] (ACGIH) NDMA,,,, N,N-,, [4,5],,,, [4-7] N,N-,, ( TEA), GB/T N- [8] (30~200 g) N,N-, D 6 -N,N-,,, [9,10],,,,,, N,N- 2 材料与方法 2.1 仪器与试剂 : - DSQ(Thermo, USA); TDL-5-A ( ); AE200 ( METTLER ); SILICA/PSA ( 1.0 g/6 ml)( ) : N,N- (1 mg/ml), ; D 6 -N,N- (1 mg/ml), Cambridge : (, Fisher ); (, ) 2.2 样品前处理 50 ml, 5 min, 10 ml 50 ml, 100 μl D6-N,N- (2.0 mg/l),, 3.0 g, 15 ml, 30 s, 10 min, r/min 4 min,,,, 1 ml, 10 g,, 40 ml, 10 min, r/min 4 min,,, 1 ml, SILICA/PSA (1.0 g/6 ml), 5 ml 5 ml,, 5 ml 10% /, 5 ml,, 1.0 ml, - (gas chromatographymass spectrometry, GC-MS), 2.3 气相色谱质谱条件 : : ( ), DB-INNOWAX (30 m 0.25 mm 0.25 µm), : 1.0 ml/min; : 250, : 1 μl, ; : : 35, 3 min, 10 /min 120, 15 /min 200, 250, 5 min : : 280 ; : 230 ; : (EI); : (SIM), 标准储备液和标准溶液的配制 N,N-,,, ( ng/ml), 200 ng/ml

2 样品前处理 50 ml, 5 min, 10 ml 50 ml, 100 μl D6-N,N- (2.0 mg/l),, 3.0 g, 15 ml, 30 s, 10 min, 10000 r/min 4 min,,,, 1 ml, 10 g,, 40 ml, 10 min, 10000 r/min 4 min,,, 1 ml, SILICA/PSA (1.

3 Table 1 表 1 N,N- 二甲基亚硝胺监测离子 Monitoring ions of N-dimethyl nitrosamine (min) 9.80 N,N- 42, D6-N,N 结果与讨论 3.1 方法的线性范围和检出限, ng/ml N,N-, N,N-, Y= X, r= N,N- ( 100 ng/ml) Fig. 2 The chromatogram of N-dimethyl nitrosamine spiking in beers at 100 ng/ml 1 N,N- (200 ng/ml) Fig. 1 The chromatogram of N-dimethyl nitrosamine standard solution (200 ng/ml) 3.2 回收率和精密度,,,, 6, 2, 72.9%~103.4%, (RSDs) 2.5%~7.7%,, 3.4 实际样品测定 N,N-, 30, N,N- 8 N,N-, 2, 2.5 μg/kg 2.8 μg/kg, N,N- (3 μg/kg)

9995 1 2 2 N,N- ( 100 ng/ml) Fig. 2 The chromatogram of N-dimethyl nitrosamine spiking in beers at 100 ng/ml 1 N,N- (200 ng/ml) Fig.

4 10, : N,N 表 2 测定 N, N- 二甲基亚硝胺的准确度和精密度 Table 2 Accuracy and precision for N-dimethyl nitrosamine ±RSD(%, n=6) 2.5 µg/l 66.9± µg/l 72.9± µg/l 82.2±4.1 2 µg/kg 74.3± µg/kg 87.5± µg/kg 103.4± µg/l 1.5 µg/l 0.60 µg/kg 2.0 µg/kg, [11] 72 N-, N,N- 83.9%, 7 μg/kg [12] 20 N,N- (NDMA) μg/kg, 60%~70%, N,N-,,,, 4 结论 N,N- -,, N,N- N,N-,,, [9], N,N- 参考文献 [1],,,. [J]., 2005, 34: Lin K, Yu SJ, Zhang JJ, et al. Study on N-nitroso compound in food and its relevant risk factors for esophageal cancer [J]. J Hyg Res, 2005, 34: [2],. N- [J]., 2011, 32: Sun WQ, Ma LZ. The online detection of N-nitrosamine of preserved ham [J]. Food Res Devel, 2011, 32: [3],,,. GC-MS N- [J]., 2012, 08(4): Wu YY, Liu FJ, Li LH, et al. Determination of optimization of N-nitrosamines in salted fish by gas chromatography-mass spectrometry [J]. South China Fish Sci, 2012, 8(4): [4],,,. SDE-GC N- [J]., 2004, 23: Zhang TZ, Tao YF, Huang HL, et al. Determination of N-nitrosamines in beer samples by single drop-extraction gas chromatography [J]. Chin J Anal Lab, 2004, 23: [5],,. GC-LRMS 3 N- [J]., 2011, 30: Zhao YX, Wang X, Hu YM. Determination of three nitrosamines in beer by GC-LRMS [J]. Chin J Anal Lab, 2011, 30: [6],,,. - / N- [J]., 2014, 32(4): Peng QR, Tang T, Yu SX, et al. Determination of N-nitrosodimethylamine in beer by frozen zone melting liquid-liquid extraction/gas chromatography [J]. Chin J Chromatogr, 2014, 32(4): [7],,. N- SPME-GC-MS [J]., 2003, 22: Tao YF, Huang HL, Zhang TZ. Determination of volatile N-nitrosocompounds in beer by SPME-GC-MS [J]. J Instrum Anal, 2003, 22: [8] GB/T N- [S]. GB/T Method for determination of N-nitrosamines in foods [S]. [9]. N- [J]., 2006, 15(4):

78 μg/kg, 60%~70%, N,N-,,,, 4 结论 N,N- -,, N,N- N,N-,,, [9], N,N- 参考文献 [1],,,. [J]., 2005, 34: 350 352. Lin K, Yu SJ, Zhang JJ, et al.

5 Weng QX. Determination of the content of N-dimethyl nitrosamine by gas chromatography-mass spectrometry [J]. Fujian Anal Test, 2006, 15(4): [10],,. GC-MS N- [J]., 2014, 8: Feng XJ, Gong H, Zhang XL. Determination of N-dimethylnitrosamine in various food by GC-MS method [J]. Sino-foreign Food Ind, 2001, 28: [11],,. N- [J]., 2001, 28: Duan FM, Chen KL, Luo HD. Study on the content of N-nitroso compound in beer, soy sauce and sausage [J]. Mod Prev Med, 2001, 28: [12],,,. [J]., 2003, 9: Li YM, Chen LR, Xue QJ, et al. Determination and analysis of N-nitroso-compounds of pickles in Wuwei city of Gansu province [J]. Anal Test Technol Instrum, 2003, 9: 作者简介 ( 责任编辑 : 杨翠娜 ) 刘印平, 硕士, 中级技师, 主要研究方向为食品安全检测 liuyinping0930@163.com 杨立新, 博士, 中级技师, 主要研究方向为食品安全检测 yanglixin241@163.com

Study on the content of N-nitroso compound in beer, soy sauce and sausage [J]. Mod Prev Med, 2001, 28: 27 28. [12],,,. [J]., 2003, 9: 88 90. Li YM, Chen LR, Xue QJ, et al.

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 蔡伟江 *, 邓鹏飞, 刘光兰, 李丹 (, 519040) 摘要 : 目的, 方法 (4.6 mm 250 mm, 5.0 μm) ; : : : =70: 16: 14(V:V:V),, : 1.0 ml/min; : 40 ; : 10

Microsoft Word 刘印平-二校 出3836-

Microsoft Word 刘印平-二校出3836-