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, R_S/N = 3) was 2 µg/kg and the limit of quantitation (LOQ, R_S/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.

A reversed-phase high performance liquid chromatographic (HPLC) method was established for the determination of erythrosine in fermented milk. After enzymatic hydrolysis, the sample was extracted with anhydrous ethanol, and purified by solid phase extraction using an HLB column under alkaline conditions. The separation was performed on a C₁₈ reverse-phase column by gradient elution using a mobile phase comprising 20 mmol/L ammonium acetate buffer solution (pH 6.5) and methanol. The detection wavelength was set at 520 nm, and quantification was performed by the external standard method. The results showed that the linear range for erythrosine was 0.05–20.00 μg/mL. The limit of quantitation (LOQ) and the limit of detection (LOD) of erythrosine in fermented milk samples were 0.2 and 0.1 mg/kg, respectively. The recoveries from fermented milk samples spiked at levels of 0.2–2.0 mg/kg were 96.5%–105.6%, and the relative standard deviations (RSD) were 1.87%–2.21%. The method is simple and accurate, has high recovery and good repeatability, and is suitable for the determination of erythrosine in fermented milk.

The measurement uncertainty was estimated for the determination of 1-oleic-2-palmitic-3-linoleic acid triglyceride (OPL) content in milk powder by gas chromatography (GC). According to the Measurement and Expression of Uncertainty in Measurement (JJF 1059.1—2012) and the Guidance on Quantifying Uncertainty in Chemical Analysis (CNAS-GL 006: 2019), a mathematical model was established to analyze the sources of measurement uncertainty. The major factors affecting the measurement uncertainty were evaluated. Results showed that the average OPL content of six milk powder samples was measured to be 1.172 g/100 g. The relative expanded uncertainty (u_rel) was 0.0236 with a coverage probability of approximately 95%. The standard uncertainty arising from sample preparation was the main source of uncertainty.

A high performance liquid chromatographic (HPLC) method was developed for the determination of naringin in milk and dairy products. Samples were extracted with methanol, and the analytes were separated on a C₁₈ column using a mobile phase consisting of 0.1% acetic acid aqueous solution and acetonitrile (75:25, V/V), detected by a diode array detector at 284 nm and quantified by an external standard method. The results showed that the linearity of this method was good in the concentration range of 5–500 μg/mL with a correlation coefficient of 0.9999. The recoveries of powdered and liquid milk power and yogurt spiked at 0.02, 0.04, and 0.08 g/100 g were 96.2%–103.2%, 96.3%–103.7%, and 99.7%–104.1%, respectively, with relative standard deviations (n = 6) of 1.12%–2.31%, 1.25%–1.85%, and 1.24%–1.66%, respectively. The reported method is simple, rapid, accurate, repeatable, and suitable for the determination of naringin in milk and dairy products.

Being rich in nutrients, dairy products provide a good environment for the growth of Staphylococcus aureus, Salmonella, Listeria monocytogenes, Cronobacter and other foodborne pathogens, which poses a serious threat to the safety of dairy products. Therefore, rapid and accurate detection of foodborne pathogens in dairy products is essential to the prevention of foodborne pathogens. In recent years, analytical techniques including molecular biology and immunoassays have rapidly developed and attracted much attention due to their advantages of high sensitivity, rapidity and simplicity compared with the traditional food pathogen detection methods, which are cumbersome and time-consuming. In this paper, recent developments and applications of foodborne pathogen detection techniques are reviewed, and future trends were discussed in order to provide a reference for the rapid detection of foodborne pathogens in dairy products.

A small amount of bacterial spores with strong tolerance still exist in raw milk after sterilization and can multiply under certain conditions, causing a serious impact on product quality and consumer health. In this study, raw milk samples containing Bacillus were collected to isolate aerobic Bacillus and thermophilic aerobic Bacillus. The isolates obtained were identified based on their morphological, physiological, biochemical and molecular biological characteristics, and the heat resistance of the isolated thermophilic aerobic Bacillus was studied. Results showed that 10 strains of Bacillus were isolated from the milk samples, of which three were thermophilic aerobic Bacillus and seven were aerobic Bacillus. Among them, Bacillus coagulans and Bacillus clausii could tolerate heat treatment at 115 ℃ for 15 min. All Bacillus in raw milk could be killed by heat treatment at 121 ℃ for 20 min which decreased the number of spores by four orders of magnitude. The dominant Bacillus species in raw milk were Bacillus subtilis, Bacillus cereus, Bacillus pumilus, Bacillus licheniformis, Bacillus circulans, Bacillus gelatini, Bacillus amyloliquefaciens, Bacillus coagulans, and Bacillus clausii. Bacillus coagulans and Bacillus clausii had stronger heat resistance and could tolerate heat treatment at 115 ℃ for 15 min.

A gas chromatographic (GC) method for the determination of 1-oleic-2-palmitic-3-linoleic-triglyceride (OPL) in milk powder was established. The samples were extracted with ether and petroleum ether, and the extract was concentrated to near dryness, re-dissolved in n-heptane, separated on a CP-TAP CB elastic quartz capillary column, detected by a hydrogen flame ionization detector, and quantified by an external standard method. The column temperature was programmed to rise. The inlet temperature was set at 330 ℃. The samples (1.0 μL) were injected using the split mode (1:10). The detector temperature was set at 360 ℃. Nitrogen was used as the carrier gas. The makeup flow rate (nitrogen) was 25 mL/min. The recovery of OPL from spiked milk powder at 1–6 g/100 g ranged from 95.2% to 101.9%, and the relative standard deviations (RSDs) for precision ranged from 1.289% to 1.998%. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method were 0.2 and 1.0 g/100 g, respectively. This method, therefore, is simple, accurate, repeatable, and suitable for the determination of OPL in milk powder.

A gas chromatographic (GC) method to determine the contents of 16 trans fatty acids in ice cream was established. The 2.0 g samples were pretreated sequentially with 8 mL of hydrochloric acid and 10 mL of anhydrous ethanol, separated on an SP-2560 capillary column, detected by GC with a flame ionization detector (FID) and quantified by the peak area normalization method. Under optimized chromatographic conditions, the limit of detection and limit of quantification of the proposed method were 0.012% and 0.024%, respectively, and it allowed effective separation of trans fatty acid methyl esters from cis fatty acid methyl esters and saturated fatty acid methyl esters.

Using multi-walled carbon nanotubes (MWCNTs) as a novel sorbent and a new special anionic chromatographic column for pesticide residues, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous direct determination of glufosinate ammonium and its metabolites 3-methylphosphino-propionic acid and N-acetylglufosinate ammonium in milk. The samples were extracted with methanol, cleaned up using MWCNTs, and degreased by high-speed centrifugation at low temperature. The analytes were separated on an Anionic Polar Pesticide (2.1 mm × 100 mm, 5 μm) column using a mobile phase containing 0.9% formic acid solution (A) and 0.9% formic acid solution-acetonitrile (B). The instrument was operated in the negative ion scanning mode with multiple reaction monitoring. Glufosinate ammonium was quantified by an internal standard method, and its two metabolites by an external standard method. The calibration curves for glufosinate ammonium and its two metabolites were linear in the concentration range of 1–50, 2–50 and 2–50 μg/L with correlation coefficient (R²) greater than 0.99. For these compounds, the limits of detection were 2.5, 5.0 and 5.0 μg/kg, and the limits of quantification were 5.0, 10.0 and 10.0 μg/kg, respectively. The recoveries ranged from 79.35% to 101.80%, with relative standard deviation (RSD) between 1.15% and 8.63%. The proposed method is characterized by simple pretreatment, stable chromatographic conditions, low impurity interference, high sensitivity and good accuracy, and is suitable for the determination of glufosinate ammonium and its metabolite residues in milk.

The proteases in cow’s milk have a great influence on the flavor and quality, especially on the shelf life of dairy products, but there is no uniform reference standard for the detection of protease activity in dairy products. This paper elaborates the sources, types and characteristics of protease in cow’s milk, and summarizes recent progress in the detection of the activity of different types of protease in cow’s milk, pointing out that the precise detection of protease activity in milk has great significance for dairy production and quality assurance.