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Determination of 26 Inorganic Elements in Dairy Products by Inductively Coupled Plasma-Tandem Mass Spectrometry
LIU Linan, WANG Yan, WU Chunmin, WANG Fang, GAO Zhuo, CAO Meng, YANG Linlin, ZHANG Chunlin, HUANG Jianhui
Journal of Dairy Science and Technology    2024, 47 (4): 19-24.   DOI: 10.7506/rykxyjs1671-5187-20240531-039
Abstract88)   HTML4)    PDF (2072KB)(56)       Save
An inductively coupled plasma-tandem mass spectrometry (ICP-MS/MS) method was established for the analysis of 26 inorganic elements in dairy products. Under MS/MS conditions, the 26 elements were detected in the no gas, collision gas (He) or reaction gas (H2, O2, NH3/He) mode and the optimal mode was selected for each of the elements. The results showed that calibration curve with good linearity was obtained for each element in the appropriate detection mode with a correlation coefficient greater than 0.999 0. The detection limits of the 26 inorganic elements ranged from 0.000 033 61 to 0.043 71 mg/kg. The spiked recoveries were between 95.50% and 104.21%, with a relative standard deviation (RSD) ≤ 3.94% (n = 11). The contents of Na, Mg, K, Ca, P, Fe and Zn were higher and the contents of the heavy metal elements Cr, As, Cd and Pb were lower in six kinds of dairy products, all of which were lower than the national standard limits. The method was characterized by simple pretreatment, high sensitivity, low limit of detection and high accuracy and could be used for the detection of inorganic elements in dairy products.
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Quantitative Determination of Fumonisin Residues in Milk and Milk Powder by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
MO Nan, ZHANG Lijia, GAO Yujie, BAI Yanmei, WANG Yang, LIU Lijun, LI Cuizhi
Journal of Dairy Science and Technology    2023, 46 (6): 34-39.   DOI: 10.7506/rykxyjs1671-5187-20231201-058
Abstract107)   HTML1)    PDF (2579KB)(45)       Save
An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous quantitative determination of fumonisin B1 (FB1), fumonisin B2 (FB2) and fumonisin B3 (FB3) residues in milk powder and milk has been established. The samples were extracted with methanol-acetic acid (98:2, V/V), diluted, cleaned up by immunoaffinity chromatography (IAC), and blown to dryness under nitrogen. The residue was re-dissolved and detected using an electrospray ionization source (EIS) in the positive ion mode with multiple reaction monitoring (MRM) and quantitative analysis was performed by the isotope-labeled internal standard method. The limit of quantification was 10 μg/kg for FB1, FB2 and FB3 in milk powder and milk. The recoveries at spiked concentration levels of 10–400 μg/kg were 92.8%–107.5%, with relative standard deviations (RSD) of 2.0%–4.3%. The matrix effects were 96.25%–122.84%. This method was characterized by short analysis time and was suitable for the determination of fumonisin residues in different dairy products.
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Determination of Dicamba Residues in Milk by High Performance Liquid Chromatography-Tandem Mass Spectrometry
ZHANG Lijia, LIU Lijun, BAI Yanmei, WANG Yang, MO Nan, GAO Yujie, LI Cuizhi
Journal of Dairy Science and Technology    2023, 46 (3): 17-22.   DOI: 10.7506/rykxyjs1671-5187-20230407-017
Abstract102)   HTML4)    PDF (2583KB)(60)       Save
The objective of this study was to establish a method for detecting the residue of dicamba in cow milk by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with 0.5% formic acid in acetonitrile, and the extract was purified by sodium chloride salting out, and separated on an Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) by gradient elution using a mobile phase composed of acetonitrile and 0.01% formic acid aqueous solution. Identification and quantification were achieved using an electrospray ionization source in the negative ion mode with multiple reaction monitoring (MRM). Under optimized pretreatment and instrumental conditions, good linearity was observed in the concentration range of 5.0–250.0 μg/L with correlation coefficient (r) more than 0.999. The limit of detection (LOD) and limit of quantification (LOQ) of the proposed method were 5 and 10 μg/kg, respectively. The recoveries of dicamba at spiked concentration levels of 10, 20 and 200 μg/kg were 104.3%, 101.5% and 96.2% with relative standard deviations (n = 6) of 3.0%, 2.0% and 1.5%, respectively. This method is simple, accurate, repeatable, and suitable for the rapid detection of dicamba in milk.
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Determination of Nonylphenol in Milk Powder by High Performance Liquid Chromatography-Tandem Mass Spectrometry
BAI Yanmei, ZHANG Lijia, WANG Yang, LIU Lijun, XIE Ruilong, DUAN Jianhua, LI Cuizhi
Journal of Dairy Science and Technology    2022, 45 (6): 22-26.   DOI: 10.7506/rykxyjs1671-5187-20220804-048
Abstract144)   HTML0)    PDF (1821KB)(395)       Save
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of nonylphenol in milk powder. Samples were extracted with acetonitrile and cleaned up with a solid phase extraction column. The analytes were separated on a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm), detected by electrospray ionization in the multiple reaction monitoring (MRM) mode, and quantified by an external standard method. The results showed that good linearity was observed in the concentration range of 1–200 ng/mL (R2 > 0.99). The limit of detection(LOD, RS/N = 3)was 2 μg/kg and the limit of quantitation (LOQ, RS/N = 10)was 5 μg/kg. The recoveries at different spiked levels were between 81.10% and 107.39% with relative standard deviation (RSD) ranging from 1.97% to 9.73%. This method has the advantages of accurate results, small background interference, simple operation, good stability and short pretreatment time, and is useful for the detection of nonylphenol in milk powder.
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A Review of Food Safety Control and Management in the Production Process of Dairy Products
WEN Guoyan, WANG Yanlong, FU Yunshuang, ZHAO Zhen, WAN Peng, LI Cuizhi, LÜ Zhiyong
Journal of Dairy Science and Technology    2022, 45 (3): 51-57.   DOI: 10.7506/rykxyjs1671-5187-20211120-006
Abstract264)   HTML3)    PDF (1785KB)(622)       Save
Dairy products are favored by more and more consumers because of their rich nutrients and good taste, and have become an important part of consumers’ dietary structure. At the same time, the food safety of dairy products has become the focus of consumers’ attention. Therefore, controlling dairy food safety is a top priority for every dairy company. This article expounds on the food safety control measures for ensuring quality and safety in each link of the dairy product production process. To ensure the safety of milk sources, pasture construction and management and risk control during breeding activities need to be considered. The control of raw and auxiliary materials needs to be carried out by considering the acceptance system, storage of raw and auxiliary materials, and upstream supplier management and control. The control of the production process needs to be carried out from the aspects of personnel, equipment, ingredient and environmental management. In addition, this review highlights the importance of big data technology in dairy food safety risk analysis. We expect that this review will be helpful to relevant enterprises in improving their work on food safety management.
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Nutrient Analysis of Milk Powder for Schoolchildren Sold in Chinese Markets
LIAO Weiyao, MENG Liping, WANG Yanbo, FU Linglin, HAN Junhua
Journal of Dairy Science and Technology    2021, 44 (5): 7-11.   DOI: 10.15922/j.cnki.jdst.2021.05.002
Abstract254)   HTML2)    PDF (1556KB)(187)       Save
This study aimed to analyze the nutritional fortification and the distribution of energy and nutrient contents of different brands of milk powder for schoolchildren sold in Chinese markets. The daily supply of energy and nutrients from each product was calculated according to the nutritional information and recommendations for consumption on the package, and compared with the amounts recommended by the Chinese dietary reference intakes (DRIs) for schoolchildren. The results showed that the contents of vitamin C, vitamin E, vitamin B6, folic acid, docosahexaenoic acid (DHA), dietary fiber and linoleic acid varied greatly among different brands of milk powder for schoolchildren. Vitamins A, D, C, taurine and the minerals calcium, iron and zinc were fortified in more than two-thirds of the investigated samples. Based on their median nutrient contents, the milk powders provided about 12% of the energy requirements of male schoolchildren at 7–10 of age, including about 30% of the protein, vitamin C, vitamin D and iron, about 40% of the vitamin B6, calcium and zinc, and nearly 50% of the vitamin A and vitamin B2. Overall, milk powder for schoolchildren, a convenient and easily available dairy product, has nutritional advantages.
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Comparison of Micellar Electrokinetic Capillary Chromatography with Diode Array Detector (MECC-DAD) and High Performance Liquid Chromatography with Fluorescence Detector (HPLC-FLD) for Detecting Five Aflatoxins in Raw Milk
XU Mingfang, GENG Mengmeng, WANG Yang, LI Ming, CHEN Gengnan
Journal of Dairy Science and Technology    2020, 43 (2): 19-25.   DOI: 10.15922/j.cnki.jdst.2020.02.004
Abstract160)   HTML0)    PDF (3066KB)(47)       Save
A new method for detecting five aflatoxin residues in raw milk was presented using micellar electrokinetic capillary chromatography with a diode array detector (MECC-DAD). The specificity of MECC-DAD was evaluated in comparison with that of high-performance liquid chromatography with a fluorescence detector (HPLC-FLD). In the MECC-DAD method, samples were cleaned up by immunoaffinity column chromatography before separation on an uncoated fused-silica capillary column using 7.5 mmol/L borate buffer with 30 mmol/L sodium dodecyl sulfonate (pH 8.5) and 5% acetonitrile and the detection wavelength was set at 214 nm. In the HPLC-FLD method, samples were separated on a C18 column (150 mm × 4.6 mm, 5 μm) by gradient elution using a mobile phase consisting of acetonitrile and water after being cleaned up by immunoaffinity column chromatography. The analytes were detected by a fluorescence detector at 360 nm excitation wavelength and 440 nm emission wavelength. Results showed that MECC-DAD gave smoother and sharper peaks that were more symmetrical without tailing. The limits of detection of MECC-DAD and HPLC-FLD were 0.182–1.669 and 0.014–0.058 μg/L, both meeting the requirements for the determination of aflatoxin residues in raw milk. The precision of HPLC-FLD was somewhat higher than that of MECC-DAD. The recoveries of MECC-DAD and HPLC-FLD were 80.3%–137.0% and 79.6%–134.0%, respectively. When the two methods were applied to the same commercial milk samples, the P value for the deviation between the quantitative results obtained was 0.900, greater than 0.05, indicating no significant difference. In conclusion, MECC-DAD was simple, efficient and inexpensive, making it more suitable for the simultaneous determination of five aflatoxins in milk than HPLC-FLD.
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Recent Progress in Human Milk Oligosaccharides and Their Substitutes in Infant Formula
WANG Yanfei, GONG Pimin, ZHANG Lanwei
Journal of Dairy Science and Technology    2020, 43 (1): 25-32.   DOI: 10.15922/j.cnki.jdst.2020.01.006
Abstract293)   HTML4)    PDF (3041KB)(152)       Save
Human milk oligosaccharides (HMOs) are important components in human milk. Understanding the differences between non-HMOs and HMOs is fundamental to develop infant formula with improved nutritional functions making it more similar to human milk to satisfy the nutritional health of infants. This paper reviews the types and structural characteristics of HMOs and their roles in regulating the intestinal microflora, improving intestinal health and promoting immune system development. Meanwhile, the differences between the composition of oligosaccharides in mammalian milk and HMOs composition are described, as well as the characteristics and functions of oligosaccharides commonly used in infant formula. The problems associated with the application of oligosaccharides in infant formula are proposed and future prospects are discussed. We expect that this review will provide a theoretical guidance for the development of new infant formulas.
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Analysis of Cr Valence States in Milk by High Performance Liquid Chromatography Coupled with Inductively Coupled Plasma Mass Spectrometry
WU Chunmin, WANG Yan, ZHANG Chunlin, WANG Dong, ZHANG Leilei, ZHANG Yan
Journal of Dairy Science and Technology    2017, 40 (6): 29-32.   DOI: 10.15922/j.cnki.jdst.2017.06.006
Abstract126)      PDF (1763KB)(87)       Save
In this paper, Cr (Ⅲ) and Cr (Ⅵ) in milk were determined by high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A PRP-X100 cation exchange column was used. The influence of mobile phase concentration, pH value and flow rate on the degree of separation and retention time was investigated. The mobile phase selected was NH4NO3solution (0.10 mol/L, pH 7) at a flow rate of 1.0 mL/min. Under the optimized conditions, the mass spectrometric and ion interferences were eliminated by using the natural abundance ratio of 52Cr to 53Cr as reference value, and the retention time of Cr (Ⅲ) and Cr (Ⅵ) were determined to be 2.227 and 1.856 min, respectively. Good linearity was observed for Cr (Ⅲ) and Cr (Ⅵ) with correlation coefficients of 0.999 5 and 0.999 7, respectively. The detection limits were 0.015 and 0.016 μg/L, respectively. The overall recoveries for the two valence states were in range of 71.52% to 90.27%. This method proved to be useful for simultaneous analysis of different Cr valence states in milk and dairy products.
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Determination of 26 Metal Elements in Infant Formula
ZHANG Leilei, WANG Yan, ZHANG Chunlin, SHEN Lu, ZHANG Yan
Journal of Dairy Science and Technology    2017, 40 (3): 16-19.   DOI: 10.15922/j.cnki.jdst.2017.03.004
Abstract121)      PDF (1549KB)(125)       Save
Inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were compared for determining the contents of metal elements in infant formula milk powder. The limits of detection (LOD) and quantitation (LOQ) of ICP-MS were established using Sc, Rh and Bi as internal standards. Relative standard deviations (RSDs) for 26 analytes were less than 5.0%, and recoveries from spiked samples were 82.80%-110.80%. Eight metal elements could be simultaneously determined by ICP-AES, whose LOD and LOQ were slightly higher than those of ICP-MS. Furthermore, ICP-AES exhibited a good linearity and spiked recoveries in the range of 91.64%-112.73%. In the end, we concluded that both ICP-MS and ICP-AES had a high precision and a good linearity, but ICP-MS allowed the determination of a wider range of metal elements with lower LOD and LOQ.
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Quality Evaluation of Whey Cheese Incorporated with Fish Protein Powder
WANG Yan, ZHAO Shuang, LIU Xiu-he, FU Mao-run
Journal of Dairy Science and Technology    2013, 36 (6): 11-34.   DOI: 10.15922/j.cnki.jdst.2013.06.003
Abstract66)   HTML0)    PDF (1427KB)(131)       Save
A whey cheese made from whey protein concentrates incorporated with fish protein powder (FPP) was evaluated. The effects of FPP concentrations including 0.4%, 0.8%, and 1.2% on the whey cheese properties were investigated by analyzing cheese yield, texture characteristics, and digestibility. The results of this study showed that the incorporation of FPP into whey cheese enhanced the yield, texture property and digestibility of whey cheese. Thus, addition of 1.2% FPP into whey cheese is useful to improve its quality.
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