Abnormal analysis of trace elements and heavy metal over-standard in dairy products are major concerns in the dairy industry, and how to detect elements of concern in dairy products quickly and accurately has become the focus of attention. Detection of elements in milk and dairy products is a prerequisite to ensure product quality and safety. Therefore, the pretreatment and detection methods specified in the Chinese and international standards for elements in milk and dairy products are reviewed. The principle, pros and cons of each method are elaborated so as to provide a reference for the detection of elements in the dairy industry.

A method for the determination of stevioside, rebaudioside A, rebaudioside B, rebaudioside C, rebaudioside F, dulcoside A, rubusoside and steviolbioside in fermented milk by high performance liquid chromatography (HPLC) was developed and validated. The chromatographic conditions and sample pretreatment conditions were optimized. Samples were ultrasonically extracted with water for 20 min and for another 10 min after addition of 30% acetonitrile in water bath at 45 ℃. Potassium ferrocyanide and zinc acetate were added to precipitate proteins. The chromatographic separation was achieved on a C18 with gradient elution using a mobile phase consisting of sodium phosphate buffer and acetonitrile, and the analytes were detected by an ultraviolet (UV) detector at 210 nm. The results showed that the method was linear in the concentration range of 1–50 μg/mL, the limit of detection (LOD, RS/N = 3) was 3.0 mg/kg, and the limit of quantitation (LOQ, RS/N = 10) was 10.0 mg/kg. The average recoveries of all analytes spiked at 15–200 mg/kg were between 92.0% and 103.1%, with relative standard deviation (RSDs) (n = 6) less than 3.0%. This method was rapid, accurate, stable, sensitive, and suitable for the analysis of the content of steviol glycosides in fermented milk.

Sample pretreatment is a key step in element testing, which directly affects the precision and accuracy of analytical results. In order to meet the requirements for the detection of various elements, in this study, we used microwave digestion combined with inductively coupled plasma-mass spectrometry (ICP-MS) operated in the collision reaction mode to determine the content of multiple elements in milk powder, and investigated the influence of sample pretreatment conditions (acid removal time, sample size, and the amount of residual acid) on the detection results. Compared to removing acid mist only, better results were obtained under the following conditions: acid removal temperature was 160 ℃, acid removal time was 97.5 min, and sample size was 0.250 0 g, and the amount of residual acid was 1.0 mL. This pretreatment process is characterized by good stability, high precision and high accuracy.

Inductively coupled plasma-mass spectrometry (ICP-MS) was used to measure the aluminum content in the quality control sample of milk powder, and an X-control chart was established for runaway judgement and handling during the operation process. The precision and median line of the control chart for new data points obtained one year later were evaluated using Minitab software with test for equal variance and analysis of variance. The standard deviation for the previous 25 data points was 0.186 mg/kg compared to 0.126 mg/kg for the 35 new ones, while the median values of the two groups did not differ from each other. More reliable control limit was calculated based on all the data points, and the new median value was 1.334 mg/kg with a standard deviation of 0.154 mg/kg. The decrease in standard deviation suggested that the precision was improved with smaller data fluctuations. In conclusion, calculation of new and more reliable control limit from more data is useful to find obvious systematic errors, abnormal data and slow changing trend in a timely and effective way and can provide evidence to decide whether data should be retained or removed so as to directly reflect the stability and tendency of the detection.

A spectrophotometric method for the determination of tea polyphenols in milk tea powder was developed by using Folin-phenol reagent. Crucial operating parameters such as extraction reagent, number of extraction cycles, temperature and derivatization reagent were investigated. Extraction using 70% methanol solution as the extraction reagent in a hot water bath at 70 ℃ performed twice and oxidization of the resulting extract with Folin-phenol reagent proved optimal. The detection wavelength was selected as 765 nm, and gallic acid was used as the calibration standard for the quantitation of tea polyphenols. The recoveries for whole milk powder spiked at concentration levels of 850–4 500 mg/kg were in the range of 98.9%–104.9%. Good stability and accuracy were achieved. When milk tea powder samples with different contents of tea polyphenols were detected in six replicates, relative standard deviations (RSDs) of 0.29%–0.84% were obtained, indicating good precision. This method proved to be accurate, easy to operate and repeatable with simple and easily available instruments, and thus suitable for the analysis of tea polyphenols in milk tea powder.

By analyzing some factors involved in the determination of lead in milk powder by inductively coupled plasma mass spectrometry (ICP-MS) such as containers and reagents used, an ultrasonic cleaning method was established to effectively reduce the blank value. The method gave a detection limit of 0.005 mg/kg, which was much lower than that (0.02 mg/kg) of traditional methods. The recoveries of samples spiked at concentration levels of 0.005–0.015 mg/kg ranged from 86.9% to 119.0% with relative standard deviations (RSDs) of 3.1%–12.3%, meeting the requirements for methodological validation. Hence, the method proved to be overall feasible and suitable for the detection of lead in milk powder with reduced detection limit.

Inductively coupled plasma emission spectrometry (ICP-OES) was used to determine the contents of 12 trace elements (K, Na, Ca, Mg, Fe, Zn, Cu, Mn, P, Sr, Al, and Cr) in premixed feed and crude feed for dairy cows. Samples were pretreated with microwave digestion before being analyzed. The calibration curves of all elements were linear with correlation coefficients above 0.999 8. The spiked recoveries for this method were 90.0%–106.9%, and the coefficients of variance (CV) for six replicate determinations were 0.69%–8.70%. With the advantages of low limits of detection and high sensitivity and accuracy, this method could be useful for the simultaneous determination of multiple trace elements in dairy feeds.