Abstract
Objective: A rapid method was established for the simultaneous determination of variety anions in liquid milk. Methods: The macromolecular protein in liquid milk was precipitated by acetonitrile, and a variety of anions were extracted. After purification by C18 column, the material was separated by Dionex IonPac AS19-HC ion column with gradient elution of potassium hydroxide and conductivity detection. Finally, a method for the determination of bromate, thiocyanate, nitrite, nitrate, chlorate, perchlorate, phosphate and iodine ion in liquid milk was established using ion chromatograph. Results: The results showed that the correlation coefficients (R2)of eight kinds of anion range from 0.999 0 to 0.999 8 in the linear range, and the limits of detection were between 0.065 mg/kg and 0.417 mg/kg. The recoveries were in the range 81.8%~102.0% with the relative standard deviations in the range 1.1%~6.7%(n=6). Conclusion: The method has the advantages of simple operation, high accuracy and sensitivity, and can be used for simultaneous determination of various anion residues in liquid milk.
Publication Date
12-26-2023
First Page
56
Last Page
61,68
DOI
10.13652/j.spjx.1003.5788.2023.60004
Recommended Citation
Ziling, WU; Xiaoqing, YAO; Yingtao, SHEN; Jiale, HUANG; and Minheng, HE
(2023)
"Determination of eight anions in liquid milk,"
Food and Machinery: Vol. 39:
Iss.
10, Article 8.
DOI: 10.13652/j.spjx.1003.5788.2023.60004
Available at:
https://www.ifoodmm.cn/journal/vol39/iss10/8
References
[1] 李媛, 刘芳. 我国乳制品行业发展现状及趋势分析[J]. 中国畜牧杂志, 2019, 55(4): 144-147.
LI Y, LIU F. Development status and trend analysis ofdairy industry in China[J]. Chinese Journal of Animal Science, 2019, 55(4): 144-147.
[2] 刘广琛. 我国乳品质量安全存在的主要问题及对策分析[J]. 中国食品, 2021(19): 90-91.
LIU G C. Analysis on the main problems and countermeasures of dairy quality safety in China[J]. China Food, 2021(19): 90-91.
[3] 左丽娜, 高腾, 张丽敏, 等. 我国乳品质量安全保障体系的建立与完善研究[J]. 食品安全导刊, 2021(6): 23, 26.
ZUO L N, GAO T, ZHANG L M, et al. Research on establishment and improvement of dairy product quality and safety assurance system in China[J]. China Food Safety Magazine, 2021(6): 23, 26.
[4] 董彬. 我国原奶及乳制品质量安全管理简述[J]. 食品安全导刊, 2019(33): 10.
DONG B. Quality and safety management of raw milk and dairy products in China[J]. China Food Safety Magazine, 2019(33): 10.
[5] 张立平. 乳制品质量安全监管的国际经验与启示[J]. 食品与机械, 2021, 37(4): 87-90.
ZHANG L P. International experiences and inspirations of dairy product safety and quality supervision[J]. Food & Machinery, 2021, 37(4): 87-90.
[6] 蓝小飞, 谢琳. 乳粉中磷含量检测的不确定度比较[J]. 食品安全质量检测学报, 2020, 11(1): 231-235.
LAN X F, XIE L. Comparison of uncertainty in determination of phosphorus content in milk powder[J]. Journal of Food Safety and Quality, 2020, 11(1): 231-235.
[7] 张梦晗, 陈宏, 封丽, 等. 食品中磷酸盐检测技术研究进展[J]. 食品工业科技, 2015, 36(19): 395-399.
ZHANG M H, CHEN H, FENG L, et al. Advances in the detection of phosphate in food[J]. Science and Technology of Food Industry, 2015, 36(19): 395-399.
[8] 陈景周, 李樑, 黄少漫, 等. 高压离子色谱法快速测定饮用水中溴酸盐和亚硝酸盐[J]. 食品与机械, 2020, 36(7): 63-66.
CHEN J Z, LI D, HUANG S M, et al. Quickly determination of bromate and nitrite in drinking water by high pressure ion chromatography[J]. Food & Machinery, 2020, 36(7): 63-66.
[9] 王小芳, 樊继彩, 任韧. 高效液相色谱—荧光检测法测定婴幼儿奶粉中的亚硝酸盐[J]. 中国卫生检验杂志, 2021, 31(7): 808-810, 816.
WANG X F, FANG J C, REN R. Determination of nitrite in infant milk powder by high-performance liquid chromatography-fluorescence detection[J]. Chinese Journal of Health Laboratory Technology, 2021, 31(7): 808-810, 816.
[10] 李华丽, 蔡楚勇. 离子色谱法测定奶粉中亚硝酸盐含量的优化[J]. 广东化工, 2021, 48(13): 195-196.
LI L H, CAI C Y. Optimization of determination of nitrite content in milk powder by ion chromatography[J]. Guangdong Chemical Industry, 2021, 48(13): 195-196.
[11] CHAMANDUST S, MEHRASEBI M R, KAMALI K, et al. Simultaneous determination of nitrite and nitrate in milk samples by ion chromatography method and estimation of dietary intake[J]. International Journal of Food Properties, 2016, 19(9): 1 983-1 993.
[12] 钟莺莺, 陈平, 俞雪钧, 等. 改进的离子色谱法测定乳制品中亚硝酸盐和硝酸盐[J]. 色谱, 2012, 30(6): 635-640.
ZHONG Y Y, CHEN P, YU X J, et al. Determination of nitrite and nitrate in dairy products by improved ion chromatography[J]. Chinese Journal of Chromatography, 2012, 30(6): 635-640.
[13] 刘桂贤, 曾家源. 离子色谱法测定饮用水中的溴酸盐[J]. 广东化工, 2018, 45(2): 176, 184.
LIU G X, ZENG J Y. Determination of bromate in drinking water by ion chromatography[J]. Guangdong Chemical Industry, 2018, 45(2): 176, 184.
[14] 李朦, 于泓, 郑秀荣. 离子色谱—紫外检测法同时分析碘酸根,碘离子,溴酸根和溴离子[J]. 色谱, 2014, 32(3): 299-303.
LI M, YU H, ZHENG X R. Simultaneous analysis of iodate, iodide, bromate and bromine ions by ion chromatography-UV detection[J]. Chinese Journal of Chromatography, 2014, 32(3): 299-303.
[15] 刘欣. 使用离子色谱法测定次氯酸钠中氯酸盐、亚氯酸盐[J]. 化工设计通讯, 2018, 44(2): 195.
LIU X. Determination of chlorite and chlorite in sodium hypochlorite by ion chromatography[J]. Chemical Engineering Design Communications, 2018, 44(2): 195.
[16] 周晓晴, 吕小丽, 万建春, 等. 高效液相色谱—串联质谱法测定奶粉中氯酸盐和高氯酸盐[J]. 色谱, 2019, 37(10): 1 064-1 070.
ZHOU X Q, LU X L, WANG J C, et al. Determination of chlorate and perchlorate in milk powder by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2019, 37(10): 1 064-1 070.
[17] 董恒涛, 张亚锋, 艾芸, 等. 超高效液相色谱—串联质谱法测定婴幼儿配方奶粉中的高氯酸盐和氯酸盐残留[J]. 食品安全质量检测学报, 2021, 12(16): 6 522-6 527.
DONG H T, ZHANG Y F, AI Y, et al. Determination of perchlorate and chlorate residues in infant formula by ULTRA performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality, 2021, 12(16): 6 522-6 527.
[18] 朱伟, 宁啸骏, 秦宇. 离子色谱串联质谱法测定婴幼儿配方奶粉中氯酸盐和高氯酸盐[J]. 食品安全质量检测学报, 2019, 10(11): 3 474-3 480.
ZHU W, NING X J, QING Y. Determination of chlorate and perchlorate in infant formula by ion chromatography-tandem mass spectrometry[J]. Journal of Food Safety and Quality, 2019, 10(11): 3 474-3 480.
[19] 李彦国, 赵莹, 张娟, 等. 碘缺乏和碘过量的流行状况及其对人体的危害分析[J]. 世界最新医学信息文摘, 2016, 16(65): 162.
LI Y G, ZHAO Y, ZHANG J, et al. Prevalence of iodine deficiency and iodine excess and its harm to human body[J]. World Latest Medicine Information, 2016, 16(65): 162.
[20] 朱伟, 宁啸骏, 秦宇. 离子色谱串联质谱法测定婴幼儿配方奶粉中氯酸盐和高氯酸盐[J]. 食品安全质量检测学报, 2019, 10(11): 3 474-3 480.
ZHU W, NING X J, QIN Y. Determination of chlorate and perchlorate in infant formula milk powder by ion chromatography tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2019, 10(11): 3 474-3 480.
[21] 刘珈伶, 郭雯雯, 韦环, 等. 离子色谱—电导法同时测定奶粉中碘离子和硫氰酸根离子[J]. 中国食品添加剂, 2018(6): 173-179.
LIU J L, GUO W W, WEI H, et al. Simultaneous determination of iodide and thiocyanate ions in milk powder by ion chromatography-conductivity method[J]. China Food Additives, 2018(6): 173-179.
[22] 韦昱, 方从容, 赵云峰, 等. 分散微固相萃取/超高效液相色谱—高分辨质谱法测定茶叶中高氯酸盐[J]. 分析测试学报, 2021, 40(4): 583-588.
WEI Y, FANG C C, ZHAO Y F, et al. Determination of perchlorate in tea by dispersive microsolid phase extraction/ultra-high performance liquid chromatography-high resolution mass spectrometry[J]. Journal of Instrumental Analysis, 2021, 40(4): 583-588.
[23] 詹胜群, 张浩, 周钧, 等. 超高效液相色谱—串联质谱法测定婴幼儿配方乳粉中氯酸盐和高氯酸盐[J]. 食品科技, 2022(1): 312-318.
ZHAN Q S, ZHANG H, ZHOU J, et al. Determination of chlorate and perchlorate in infant formula milk powder by ultra performance liquid chromatography-tandem mass spectrometry[J]. Food Science and Technology, 2022(1): 312-318.
[24] 梁志森, 岑建斌, 区硕俊. 同位素稀释超高效液相色谱—串联质谱法同时测定液态乳中的高氯酸盐和氯酸盐[J]. 当代化工, 2019, 48(7): 1 619-1 622.
LIANG Z S, CEN J B, OU S J. Simultaneous determination of perchlorate and chlorate in liquid milk by isotope dilution ultra-high performance liquid chromatography tandem mass spectrometry[J]. Contemporary Chemical Industry, 2019, 48(7): 1 619-1 622.
[25] 刘丽菁, 杨艳, 张文婷, 等. 离子色谱法测定饮用水中高氯酸盐残留量[J]. 中国预防医学杂志, 2019, 20(12): 1 150-1 153.
LIU L J, YANG Y, ZHANG W T, et al. Determination of perchlorate residue in drinking water by ion chromatography[J]. Chinese Journal of Preventive Medicine, 2019, 20(12): 1 150-1 153.
[26] PAUN I, IANCU V I, CHIRIAC F L, et al. New ion-chromatography method for detection of chlorite, chlorate, and bromate in drinking water[J]. Romanian Journal of Ecology & Environmental Chemistry, 2020, 2(2): 49-55.
[27] 钱冲, 勾新磊, 史迎杰, 等. 气相色谱法测定婴幼儿配方奶粉和母乳中的碘[J]. 食品安全质量检测学报, 2018, 9(15): 4 061-4 065.
QIAN C, GOU X L, SHI Y J, et al. Determination of iodine in infant formula and breast milk by gas chromatography[J]. Journal of Food Safety & Quality, 2018, 9(15): 4 061-4 065.
[28] 相萍萍, 徐书杭, 刘超. 食物中碘的测定方法[J]. 中国食物与营养, 2017, 23(10): 34-37, 41.
XIANG P P, XU S H, LIU C. Method for the determination of iodine in food[J]. Food and Nutrition in China, 2017, 23(10): 34-37, 41.
[29] 樊祥, 陈迪, 张润何, 等. 微波消解—电感耦合等离子体质谱法测定乳制品中总碘[J]. 理化检验(化学分册), 2015, 51(1): 119-121.
FAN X, CHEN D, ZHANG R H, et al. Determination of total iodine in dairy products by microwave digestion and inductively coupled plasma mass spectrometry[J]. Phys Test Anal (Part B: Chem Anal), 2015, 51(1): 119-121.
[30] 丁玉龙, 葛宇, 徐红斌, 等. 微波消解—电感耦合等离子体质谱法测定乳制品中总碘[J]. 分析测试技术与仪器, 2016, 22(3): 184-188.
DING Y L, GE Y, XU H B, et al. Determination of total iodine in dairy products by microwave digestion and inductively coupled plasma mass spectrometry[J]. Anal Test Technol Instrum, 2016, 22(3): 184-188.
[31] 潘灿盛, 张志舟, 夏冰, 等. 抑制电导离子色谱法测定奶酪中硫氰酸根的不确定度评定[J]. 食品与机械, 2023, 39(3): 49-54, 121.
PAN C S, ZHANG Z Z, XIA B, et al. Evaluation of uncertainty for the determination of thiocyanate in cheese by inhibited conductivity ion chromatography[J]. Food & Machinery, 2023, 39(3): 49-54, 121.
[32] 宣栋操, 朱震海, 蔡嵘. 顶空气相色谱法测定牛奶中的硫氰酸盐[J]. 中国卫生检验杂志, 2012, 22(8): 1 754-1 756.
XUAN D C, ZHU Z H, CAI R. Determination of thiocyanate in milk by headspace gas chromatography[J]. Chinese Journal of Health Laboratory Technology, 2012, 22(8): 1 754-1 756.
[33] 胡桂林, 薛志清, 张河霞, 等. 气相色谱法测定牛奶和奶粉中的硫氰酸盐[J]. 中国乳品工业, 2010, 38(10): 54-56.
HU G L, XUE Z Q, ZHANG H X, et al. Determination of thiocyanate in milk and milk powder by gas chromatography[J]. China Dairy Industry, 2010, 38(10): 54-56.