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CHEMICAL ENGINEERING JOURNAL · 2024 · IF 13.3

Sustainable 3D-printed β-galactosidase immobilization coupled with continuous-flow reactor for efficient lactose-free milk production

Yun Shao,Ni Gan,Bingbing Gao,Bingfang He

The production of low-lactose and lactose-free milk remains a critical challenge. Novel enzyme immobilization integrated with the flow reactor that could be applied to hydrolyze milk with cost-effectiveness, facilitation, and safety is highly expected. Here, we present a novel continuous-flow bioreactor loaded with β-galactosidase (β-Gal) covalently immobilized 3D-printed scaffolds for the production of lactose-free milk. 3D-printed polylactic acid (PLA) scaffolds modified by self-assembly of polyethyleneimine and sodium hyaluronate layers are rapidly branched with functional groups, followed by covalent immobilization of β-Gal using genipin as the cross-linker. The use of genipin allows efficient and stable immobilization of the enzyme (92.87 % immobilization efficiency), and the immobilized enzyme retains 90.53 % activity after 6th repeated use. Moreover, the 3D-printed scaffolds integrated into the flow reactor perturbed the fluids in the different reactors through directional channels, which improved the internal mass transfer to achieve high catalytic activity (94.20 % lactose hydrolysis efficiency). The lactose residues of milk reacted in the β-Gal flow reactor for 6 and 12 h were 1.87 g dL -1 and 0.38 g dL -1 , which fully met the requirements of the national food safety standards for low-lactose and lactose-free milk. Due to the high efficiency of enzyme immobilization and the stable catalytic activity of the reactor, it has a broad application prospect for the production of low-lactose and lactose-free milk and other biocatalytic fields.

CAS / MDL: 6902-77-8
研究领域: 食品科学 · 生物工程 · 酶技术
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SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY · 2021 · IF 4.098

SERS Detection of Benzoic Acid in Milk by Using Ag-COF SERS Substrate

Zichen Yang,Chaoqun Ma,Jiao Gu,Yamin Wu,Chun Zhu,Lei Li,Hui Gao,Wenzhi Yin,Zirui Wang,Ye Zhang,Yunpeng Shang,Chengwei Wang,Guoqing Chen

Benzoic acid, which has a pivotal role in food additive, is prohibited to add as a preservative in dairy products. China, Brazil, and other countries have proposed standard methods to detect the addition of benzoic acid in food. Surface-enhanced Raman scattering (SERS) is an upcoming spectral detection technique, which has been widely used in the field of material analysis with the advantages of non-invasive, fast detection speed and complex environment with little interference. To detect the illegal use of benzoic acid in dairy industry, we developed Ag-COF (covalent-organic framework) material as SERS substrate to detect benzoic acid in liquid milk. The great enhancement ability of Ag-COF substrate is controlled by the addition of acetic acid and complex interplay between COF material and benzoic acid. This detection method has high sensitivity and reliability that allows us to achieve limit of detection (LOD) of 0.13 μg/mL in milk and 0.00372 μg/mL in water by applying this method. In experiment on recovery rate of real samples, the detection time is less than 15 minutes and the relative standard deviation (RSD) ranged from 2.82% to 5.69%. Therefore, this method has practical significance of the detection of benzoic acid in dairy products.

CAS / MDL: 65-85-0
研究领域: 食品科学 · 分析化学 · 材料科学
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FOOD RESEARCH INTERNATIONAL · 2021 · IF 6.475

Multi-omics revealed the effects of rumen-protected methionine on the nutrient profile of milk in dairy cows

Fengfei Gu,Shuling Liang,Senlin Zhu,Jianxin Liu,Hui-Zeng Sun

Cow’s milk is a highly-nutritious dairy product part of human diet worldwide. Rumen-protected methionine (RPM) is widely used to improve lactation performance of dairy cows, but understanding of the effects of RPM on milk nutrients composition are still limited. In this study, twenty mid-lactating dairy cows were supplemented with 20 gm/day RPM for 8 weeks to investigate the responses of milk nutritional composition to RPM. Metabolomics was applied for analyzing milk metabolites and 16S rRNA gene sequencing was used for analysis of rumen microbial composition. Milk fat content and yield were significantly increased after RPM supplementation. Totally 443 compounds belonging to 15 classes were identified, among which 15 metabolites were significantly changed. The functional nutrient α-ketoglutaric acid were significantly increased in the milk after RPM supplementation. We found 48 significantly differing bacterial genera in the rumen after supplementing RPM. Multi-omics integrated analysis revealed the higher abundance of Acetobacter , unclassified_f_Lachnospiraceae and Saccharofermentan contributed to the improved milk fat. In addition, the enriched abundance of Thermoactinomyces , Asteroleplasma , and Saccharofermentan showed positive correlations with higher α-ketoglutaric acid of milk. Our results uncover the metabolomic fingerprint and the key functional metabolites in the milk after supplementing RPM in dairy cows, as well as the key rumen bacteria associated with them. These findings provide novel insights into the development of functional dairy products that enriched the functional nutrient α-ketoglutaric acid or high milk fat.

CAS / MDL: 64-18-6
研究领域: 动物营养学 · 微生物学 · 代谢组学 · 乳品科学
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FOOD CHEMISTRY · 2021 · IF 7.514

Paper-based analytical device for high-throughput monitoring tetracycline residue in milk

Huimin Lu,Miaosi Li,Azadeh Nilghaz,Lizi Li,Guangxue Chen,Yanbin Jiang,Junfei Tian

A low-cost and portable paper-based analytical device has been developed for high throughput and on-site monitoring TC residue in milk through visualized colorimetric reaction. The filtration and concentration effect induced by the porous nature of paper contribute to strengthen the color intensity, leading to quantitative and sensitive detection of tetracycline reaching 1 ppm detection limit, with the linear range of 1–100 ppm both in water and milk samples. The applicability was demonstrated by detection of TC in 18 different types of real milk samples with good recovery ranging from 88% to 113%. Furthermore, the dynamic degradation behavior of tetracycline was monitored through the device. To the best of our knowledge, this is the first report of colorimetric detection of tetracycline in milk using the paper-based device. This simple, fast, cost-effective (~$0.50 per device) and equipment-free paper-based platform provides a promising tool for future application in food and environmental safety.

CAS / MDL: 10031-43-3
研究领域: 分析化学 · 食品安全 · 环境科学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2012 · IF 2.545

Determination of melamine concentrations in dairy samples

Wei Feng,Changyin Lv,Liping Yang,Jianlin Cheng,Chengyan Yan

Melamine, a basic organic chemical intermediate, can cause renal failure because of the formation of insoluble melamine cyanurate crystals in the kidneys. This study examined a novel fluorescence spectrometry for the determination of trace melamine in dairy. The method was based on the inhibitory effect of melamine on the decolorizing reaction of the uncatalytic oxidation of acridine red by potassium permanganate in a sulfuric acid medium. The calibration graph was linear for melamine concentrations of 2.1 × 10 −4 –1.6 mg/L, and a detection limit of 61.5 ng/L was obtained. The melamine was determined in dairy samples by the proposed method after liquid–liquid and solid phase extraction. The results correlated with the high-performance liquid chromatography. The recoveries were within the range of 99.6–103.3% for liquid milk and 98.5–111.1% for milk powder. The possible mechanism of the reaction was also investigated by ultraviolet spectra.

研究领域: 分析化学 · 食品安全 · 生物医学
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EUROPEAN FOOD RESEARCH AND TECHNOLOGY · 2014 ·Vol. 238 ·期 5 ·889-894 · IF 1.387

A non-diazotization-coupling reaction-based colorimetric determination of nitrite in tap water and milk

Zhu Jinghui,Li Chunyan,Liu Shaopu,Liu Zhongfang,Yang Jidong,Tian Jing,Hu Xiaoli

A non-diazotization-coupling reaction-based colorimetric method was developed and validated for the determination of nitrite in tap water and milk samples. Under acidic condition, nitrite could selectively react with pyrrole, resulting in the emerging of a new absorption peak at 509 nm and a distinct color change from clear to red, with which the concentration of nitrite can be determined indirectly. Excellent linear range was achieved from 0.72 to 40.0 μmol L −1 with a detection limit of 0.22 μmol L −1 . The detection limit was lower than or comparable to most of the recently published methods. The experimental conditions were optimized, and effects of coexisting substances were evaluated, and the results showed excellent priority since a certain amount of other anions, including SO 3 − , SeO 3 − and other acid radicals, would not interfere with the measurement. We highlighted the simplicity and efficiency of this method as no diazotization-coupling procedure and toxic aniline were involved. Determination of nitrite in tap water and milk samples was performed.

研究领域: 分析化学 · 环境科学 · 食品科学
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FOOD CHEMISTRY · 2022 · IF 9.231

A rapid method to measure melatonin in biological fluids (milk and serum) with liquid chromatography-tandem mass spectrometry

Songyang Yao,Xuening Liu,Yao Fu,Shengyu Guan,Yunjie Liu,Laiqing Yan,Pingli He,Guoshi Liu

Since the global demanding of natural melatonin-enriched milk has been significantly increased in the populations of children and elder, the accurate and quick melatonin detection from milk is urgently required. Thus, the regular methods no longer satisfy this requirement. In the current study, we reported a novel method to extract melatonin from milk for liquid chromatography-tandem mass spectrometry melatonin detection. This novel method was to use cold methanol (-20℃) to precipitate proteins and fat in milk with one step to extract melatonin. Compared to the regular methods, it was devoid of procedures of sample drying, solid phase extraction and sample reconstitution. It could short the extraction time from the regularly 150 min to 60 min/per 24 milk samples. We believe that this novel method provides a possibility to detect large scale of milk samples in relatively short time with more efficiency and less cost compared to the regular method.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 生物医学
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SENSORS AND ACTUATORS B-CHEMICAL · 2018 · IF 5.667

Development of a highly specific chemiluminescence aptasensor for sulfamethazine detection in milk based on in vitro selected aptamers

Ling Yang,Hengjia Ni,Chenglong Li,Xiya Zhang,Kai Wen,Yuebin Ke,Huijuan Yang,Weimin Shi,Suxia Zhang,Jianzhong Shen,Zhanhui Wang

Antibody-based sensors are the most widely used for screening antibiotic residues in food samples. However, these sensors always suffer from cross-reacting antibiotics which are able to bind the employed antibodies in a manner similar to the target, thus resulting in inaccurate quantification. In this study, we developed a highly specific and sensitive chemiluminescence aptasensor for sulfamethazine (SMZ) by employing the supernormal selectivity of a new selected aptamer. Four SMZ-specific aptamers ( K d ranging from 79 to 274 nM) were selected in vitro by MB-SELEX with an intentional counter selection to avoid the recognition other sulfonamides, which is impossible to achieve in the corresponding procedure of antibody production. The binding mechanism of aptamers for SMZ was further analyzed and clarified with molecular simulation and docking. Under optimum conditions, the chemiluminescence aptasensor based on the highest affinity aptamer named SA07 provided a limit of detection of 0.92 ng/mL with negligible cross-reactivity with the 27 tested sulfonamides. The developed aptasensor was applied to milk samples, and achieved good accuracy and precision. These results demonstrated that the integration of an aptamer and chemiluminescence in a sensor platform is a promising method for the sensitive, specific, rapid and accurate detection of antibiotic residues of interest in food samples.

研究领域: 食品安全检测 · 生物传感技术
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Foods · 2025 ·Vol. 14 ·期 5 ·852 · IF 5.1

Goat Milk Exhibits a Higher Degree of Protein Oxidation and Aggregation than Cow Milk During Cold Storage

Lirong Zhu,Zixuan Fan,Wenhao Li,Yuanyuan Shan

Due to their markedly distinct protein compositions and structures, goat milk and cow milk display substantially different characteristics. In this study, the quality and composition of goat milk and cow milk were studied after being refrigerated at 4 °C for 7 days, with a particular focus on protein oxidation and aggregation states. The results revealed that alongside increases in acidity, microbial colony count, and hydrolysis, there was a significant change in the protein aggregation state beginning on the second day. This change was characterized by increased turbidity, an elevated centrifugal sedimentation rate, and a right-shifted particle size distribution. After seven days of refrigeration, the centrifugal sedimentation rate of goat milk increased from 0.53% to 0.97%, whereas that of cow milk rose from 0.41% to 0.58%. The degree of aggregation was significantly greater in goat milk compared to cow milk. Additionally, both protein and lipids exhibited substantial oxidation, with the degree of oxidation more pronounced in goat milk than in cow milk. The malondialdehyde (MDA) content increased from 0.047 μg/mL to 0.241 μg/mL in goat milk and from 0.058 μg/mL to 0.178 μg/mL in cow milk. The results suggest that goat milk was more prone to oxidation, which further reduced its stability. Therefore, in the storage and transportation of dairy products before processing, it is essential not only to monitor sanitary conditions but also to effectively control protein oxidation to enhance the quality of milk processing.

CAS / MDL: 69-78-3
研究领域: 食品科学 · 生物化学
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JOURNAL OF FOOD PROCESS ENGINEERING · 2018 ·Vol. 42 ·期 2 ·e12976 · IF 1.955

A novel on-chip solution enabling rapid analysis of melamine and chloramphenicol in milk by smartphones

Ning Yang,Liang-Liang Xie,Chen Pan,Min-Feng Yuan,Zhi-Han Tao,Han-Ping Mao

Ubiquitous food security control is desirable. However, the analysis methods, such as those for milk, are highly based on manual analysis, leading to low efficiency. Thus, we report a multilayer paper-based microfluidic chip transforming chromatic readout to electric signals. First, colloidal gold immunochromatographic assays (GICA) are used to achieve the colorimetric occurrence. Secondly, the test (T) lines and control (C) lines are patterned to encode different EAN-8 barcode. Furthermore, accurate scanning is accomplished by the automatic threshold segmentation. These technologies make the digital determination of melamine (MEL) and chloramphenicol (CAP) by phone readily accessible. Results indicate that the accurate machine-scanning can be assured when MEL and CAP is above 30 ng/mL and 6 ng/mL in milk respectively. The detection time is under 8 min, and the stable storage life is over 90 days. Therefore, this simple chip allows rapid, machine-readable, electric-recordable diagnostic directly from chromatic assays with satisfying stability, specificity and accuracy. Practical applications This article illustrates a method used to determine the concentration of melamine and chloramphenicol in milk. When melamine and chloramphenicol is above 30 and 6 ng/ml in milk, the produced EAN-8 barcode can be recognized with high accurate level, compared with international standards, the results are acceptable and sensitive. This method is highly intellectual and environmentally friendly, with the disposable materials and instant smartphone-readable EAN-8 results patterns. This article demonstrates a multilayer paper chip based on EAN-8 encoding rules, colloidal gold nanoparticles, and immunochromatographic assays. The EAN-8 format assay is achieved by color-development occurrence of colloidal GICA in different encoding areas of EAN-8 code, and the analysis device, namely smartphone, is accessible by almost every individual. Therefore, this chip can pave a potential way for massive health control and digital automated analysis for daily life and industrial manufacture.

CAS / MDL: 9005-64-5
研究领域: 食品安全 · 分析化学 · 生物医学工程
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ANALYTICAL LETTERS · 2018 · IF 1.206

Convenient Determination of Sulfamethazine in Milk by Novel Ratiometric Fluorescence with Carbon and Quantum Dots with On-site Naked-eye Detection and Low Interferences

Li Chen,Yeqing Xu,Lin Sun,Jiahong Zheng,Jiangdong Dai,Chunxiang Li,Yongsheng Yan

Sulfamethazine, one of the most widely applied feed additives, has been shown to cause negative health effects to humans. In the present work, a novel and facile fluorescence visual detection probe was established to determine sulfamethazine in milk samples with naked-eye detection. Considering the good stability, excellent optical properties, and easy synthesis, blue-emission carbon dots were used as the standard signal and red-emission CdTe quantum dots as the responsive signal for the determination of sulfamethazine. The fluorescence intensity of red-emission CdTe quantum dots was gradually quenched with increasing concentration of sulfamethazine, while the blue-emission carbon dots response remained constant. Apparent color variations were observed by naked-eye detection in the concentration range from 9.0 to 54 µmol · L−1. In addition, the presented strategy was shown to be promising to provide a rapid, facile, and sensitive method for the determination of sulfamethazine in milk samples with few interferences.

研究领域: 分析化学 · 食品科学
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JOURNAL OF COLLOID AND INTERFACE SCIENCE · 2015 · IF 3.368

Determination of melamine in powdered milk by molecularly imprinted stir bar sorptive extraction coupled with HPLC

Ling Zhu,Guanhong Xu,Fangdi Wei,Jing Yang,Qin Hu

A novel molecularly imprinted stir bar (MIP-SB) was developed with melamine (MA) as the template molecule in this study. The sorptive capacity of MIP-SB was nearly three times over that of non-imprinted stir bar (NIP-SB). The MIP-SB presented much better selectivity than NIP-SB when used to absorb MA and its analogues. An analytical method to determine MA in powdered milk was established by combining MIP-SB sorptive extraction with HPLC. The liner range was 0.0631–12.6   ng/mL with good correlation coefficient of 0.9983, and the limit of detection was 0.0127   ng/mL based on three times ratio of signal to noise. This method was successfully applied to the determination of MA in powdered milk with satisfactory results. The method built is simple and suitable for the determination of MA in milk products which is of great significance for quality control of milk products.

研究领域: 分析化学 · 食品科学
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