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1 5 7 Vol. 5 No Journal of Food Safety and Quality Jul., 2014 胡彩霞 *, 李红, 刘美霞, 任丽, 李秋琴, 王佳, 马文丽, 宋晓东 (, ) 摘要 : 目的方法,,,,, 结果 80%~110%, 90%~110%, 10% 结论,, 关键词 : ; ; ; ; ; ; ; Determination of nitrate and nitrite content in milk and dairy products using ion chromatography HU Cai-Xia *, LI Hong, LIU Mei-Xia, REN Li, LI Qiu-Qin, WANG Jia, MA Wen-Li, SONG Xiao-Dong (Inner Mongolia Mengniu Dairy Group Co. Ltd., Hohhot ) ABSTRACT: Objective To improve the pretreatment method of national standard to detect nitrate and nitrite in Milk and dairy products. Methods Samples were extracted by acetonitrile, and after protein and fat precipitation, the extract was purified by anion exchange column, potassium hydroxide solution as leached solution. Nitrate and nitrite were detected by conductivity detector. Results The recoveries of nitrate and nitrite were 80%~110% and 90%~110% respectively, and the precision of the method were within 10%. Conclusion This method can improve the detection accuracy and reduce the detection error, and is suitable for the quantitative detection of nitrate and nitrite in milk and dairy products. KEY WORDS: nitrate; nitrite; ion chromatography; pre-treatment; improvement; acetonitrile; milk; dairy products 1 引言,,,, 0.2~0.5 g,,, C E,,, GB ,,,, * 通讯作者 :,, mnwlp88@163.com *Corresponding author: HU Cai-Xia, Researcher, Inner Mongolia Mengniu Dairy Group Co., Ltd., Hohhot mnwlp88@163.com

2 2236 5,,,,,,,,,, 2 材料与方法 2.1 材料与试剂 : 18.2 Ω cm MILLIPORE : () : () : (NO 2- )(1000 mg/l, ) (NO 3- )(1000 mg/l, ) : ( NO 2-, )( NO 3-, ) : (NO 2- ) (NO 3- ) 1.0 ml 10 ml 100 ml,, NO 2- NO mg/l mg/l 2.2 仪器与设备 ():,,, 100 µl ( ) IKA IKA EImasonic : 0.1 mg Sartorius : r/min, 30 ml 50 ml 0.22 µm / : 2.5 ml 5.0 ml : C 实验方法测定步骤 (1) g(, 2 g,, 0.1 mg) 30 ml 50 ml, 5 ml, 5~10 min, 15 ml, 5 min, r/min 10 min, 5 ml, 20 ml (4 ) : 4, (2) 15 ml, 0.22 μm IC-RP, 3 ml/min, 6 ml, (IC-RP ) (3) : 1 : IonPac AS11-HC, mm ; IonPac AG11-HC, 4 50 mm( ), ; 2 : ; : KOH, 0~48 min, 3 mmol/l; 48~48.1 min, 3~50 mmol/l; 48.1~56 min, 50 mmol/l; 1.30 ml/min; ml/min; 4 : 40 ; 5 : ; 6 : ; : 100 µl 测定 (1),,, mg/l; mg/l,, (2) 100 µl,,,, (μs) 结果计算 ( NO - 2 )( NO - 3 ) :

7, : 2237 C V f 1000 X= -------------------- M 1000 : X ; C (mg/l); V (ml); f ; M (g) : 1.5, ( ) ; 1.37, ( ) [1] 2.3.4 精密度 10% 2.3.5 检出限 0.2 mg/kg 0.4 mg/kg 3 结果与讨论,, 0.01~0.1 mg/kg 0.02~0.2 mg/kg 0.05~0.

3 7, : 2237 C V f 1000 X= M 1000 : X ; C (mg/l); V (ml); f ; M (g) : 1.5, ( ) ; 1.37, ( ) [1] 精密度 10% 检出限 0.2 mg/kg 0.4 mg/kg 3 结果与讨论,, 0.01~0.1 mg/kg 0.02~0.2 mg/kg 0.05~0.5 mg/kg 0.1~1.0 mg/kg 0.15~ 1.5 mg/kg 0.2~2.0 mg/kg, R 2 3 9, 1 2 7,,, 0.22 µm,,, 回收率能达到实验既定要求,,, 改进前处理方法与原国标方法沉淀剂不同处 3%, 2 ml,,,,,,,, 3.3 提高了检测效率, 缩短了前处理时间 30 min,,, ;,,, 20~25 min 1 Fig. 1 Nitrite standard curve pattern

1%; 果见表 2 硝酸盐加标回收率为 95.9% 107.8%, 依据 GB/ 精密度检测均在 10%以内 T27404-2008,被测组分含量在 0.1 1 mg/kg 时, 回收取奶粉依据 GB5009.

4 2238 食品安全质量检测学报第5卷图 2 硝酸盐标准曲线图谱 Fig. 2 Nitrate standard curve chart patterns Fig. 3 图 3 样品测定硝酸盐和亚硝酸盐色谱图谱 Chromatogram of determination of nitrate and nitrite in the sample 本方法亚硝酸盐加标回收率为 86.8% 109.1%; 果见表 2 硝酸盐加标回收率为 95.9% 107.8%, 依据 GB/ 精密度检测均在 10%以内 T ,被测组分含量在 mg/kg 时, 回收取奶粉依据 GB 第一法样品前处理率在 80% 110%, 改进后方法回收率能满足此规定 3.4 方法重复性实验取纯牛奶依据本方法进行精密度试验, 检测结方法进行精密度试验, 检测结果见表 3 GB 第一法中, 前处理方法检测样品重复性均超出 10%的范围内

5 7, : 2239 Table 1 表 1 以纯牛奶为本底, 依据 GB/T27404 推荐加标量按照以上方法测定结果 Pure milk as substrate, the measurement results according to the above method based on GB/T27404 recommend adding scalar (g) NO 2 - % NO 3 - % / / / / / / / / Table 2 表 2 乳样重复性检测结果 Reproducible test results of milk samples m(g) C(mol/L) % Table 3 表 3 乳样重复性检测结果 Reproducible test results of milk samples m(g) C(mol/L) % 结论 :, :,,

2240 5 80%~110% : 20 min,,,,,, 参考文献 [1] GB5009.33-2010 [S]. GB5009.33-2010 National food safety standard-determination of nitrate and nitrite [S]. [2]. [M]. :, 2001: 2 4. Guo BH. Dairy chemistry [M].

Judging dairy industry market structure [J]. China Dairy Ind, 2006, 34(02): 47 50. [5] GB5009.9-2010 [S] GB5009.9-2010 National food safety standard-milk [S]. [6]. [M]. :, 1998: 256 289. Tan TN.

GBT 603-2002 Chemical reagent-preparations of reagent solutions for use in test methods [S]. [8] GBT27404-2008 [S].

6 %~110% : 20 min,,,,,, 参考文献 [1] GB [S]. GB National food safety standard-determination of nitrate and nitrite [S]. [2]. [M]. :, 2001: 2 4. Guo BH. Dairy chemistry [M]. Beijing: China Light Industry Press, 2001: 2 4. [3] GB [S]. GB People's republic of china national standard-milk test method [S]. [4]. [J]., 2006, 34: Guo SY. Judging dairy industry market structure [J]. China Dairy Ind, 2006, 34(02): [5] GB [S] GB National food safety standard-milk [S]. [6]. [M]. :, 1998: Tan TN. The principle of chemical engineering [M]. Beijing: Chemical Industry Press, 1998: [7] GBT [S]. GBT Chemical reagent-preparations of reagent solutions for use in test methods [S]. [8] GBT [S]. GBT Laboratory quality control standards of food physical and chemical detection [S]. [9] [S]. National dairy safety standards [S]. [10]. [J]., 2013, 41 (11): Zhang SP. Study on the overall situation of development of China's dairy industry market [J]. China Dairy Ind, 2013, 41(11): [11]. [J]., 2014, 47, (1): Liu Y. The influence of different precipitation method concentration of protein in milk by [J]. China Dairy Ind, 2014, 47, (1): [12] GB/T [S]. GB/T The fourth part of rules for drafting standards- methods of chemical analysis [S]. [13] GB/T A.2, A.2.2 [S]. GB/T Detection limits of A.2, Absorption method of A.2.2 [S]. [14]. [J]., 2014, (1): Luo XH. Nitrate in vegetables was determined by ultraviolet spectrophotometer [J]. J South China Univ Trop Agric, 2014, (1): [15]. [J]., 2002, (1): Dong J. The determination of nitrite by UV spectrophotometry [J]. Environ Monit China, 2002, (1): 作者简介 ( 责任编辑 : 杨翠娜 ) 胡彩霞, 研究员, 主要研究方向为乳品检测分析 mnwlp88@163.com

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.