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Rapid identification of edible quality of rice and rice noodles based on paddy raw grain quality

FOOD SCIENCE 2024, 45 (7): 0-0.

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The aging of paddy has a direct influence on its edible quality, and the requirements for the degree of aging of paddy during processing are varied according to its final eating mode. In order to determine the paddy quality indexes and the corresponding threshold interval suitable for rice or rice noodles processing, and establish a method to identify the edible quality of rice and rice noodles rapidly. In the present study, the paddy was accelerated aged and stored, and the raw grain indexes of paddy with different aged degrees and the edible quality indexes of processed rice and rice noodles were measured, meanwhile principal component analysis, cluster analysis and stepwise regression were used to process and analyze the measured data, and finally the correlation indexes were combined with the L*, a* and b* values of solution in acid-base indicator method. The color of rice and rice noodles based on raw grain quality was restored by image processing software. The results showed that the regression equation of rice comprehensive score and fatty acid value was Y = 7.729-0.236X fatty acid value. The quality of rice can be divided into excellent, medium and poor levels based on the corresponding comprehensive score ranges of Y≥ 2.361, -1.039≤Y < 2.361 and Y< -1.039, and the corresponding thresholds for fatty acid values were X fatty acid value ≤ 23 mg/100g, 23 mg/100g < X fatty acid value ≤ 37mg/100g, and X fatty acid value >37mg/100g, respectively. The regression equation between the comprehensive score and fatty acid value of rice noodles was Y= -17.030+1.021X fatty acid value -0.015X fatty acid value 2. The quality of rice noodles can be divided into excellent, medium and poor levels based on the corresponding comprehensive scores of Y≥ 0.244, -1.589≤Y < 0.244≥ -1.589 and Y< -1.589, and the corresponding thresholds for fatty acid values were 31 mg/100g ≤ X fatty acid value ≤ 37 mg/100g, 37 < X fatty acid value ≤ 45mg/100g, and X fatty acid value > 45mg/100g , respectively. The obtained colorimetric card based on fatty acid value can directly judge the suitable eating way of paddy, which provided basis and guidance for the processing of paddy raw grain.

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Rapid quantitative authentication of vegetable blend oil quality by Raman spectroscopy coupled with spectral characteristic intervals selection algorithm

Zhi-Ming GUO

FOOD SCIENCE 0, (): 0-0.

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In this study, a method for rapid and quantitative determination of the content of high-value vegetable oil in vegetable blend oils was proposed based on Raman spectroscopy and a spectral characteristic intervals selection algorithm. First, the particle swarm optimization (PSO) algorithm and the grey wolf optimization (GWO) algorithm were combined to develop a hybrid intelligent optimization algorithm, i.e., PSOGWO algorithm. Second, the PSOGWO algorithm and the combined moving window (CMW) strategy were combined to develop a novel spectral characteristic intervals selection algorithm, i.e., PSOGWO-CMW algorithm. Third, the corn oil (CO)-extra virgin olive oil (EVOO) vegetable blend oil was prepared by mixing CO and EVOO with different ratios, and then the Raman spectra of CO-EVOO vegetable blend oil were measured. To investigate the performance of PSOGWO-CMW, the PLSR, PSO-CMW, GWO-CMW, and PSOGWO-CMW models were applied on the Raman spectra of CO-EVOO vegetable blend oil to predict the content of EVOO, and their prediction results were comparatively studied. The results showed that PSOGWO-CMW model possessed superior prediction performance. Finally, the proposed method and the gas chromatography-mass spectrometry method were employed to determine the content of EVOO in real CO-EVOO vegetable blend oils, respectively. The results showed that there was no significant difference between these two methods. In conclusion, the proposed method is rapid and accurate, and it can also be used for rapid and quantitative determination of the content of high-value vegetable oil in other vegetable blend oils.

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A sandwich immunosorbent assay for the small molecule compound 3-Amino-2-oxazolidinone based on derivatization

feng ronghu

FOOD SCIENCE 0, (): 0-0.

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urazolidone [N-(5-nitro-2-furfurylidenenamino)-2-oxazolidinone] is a member of the nitrofuran antibiotics family which are often abused in animal farming. Its metabolite, 3-Amino-2-oxazolidinone (AOZ), is a small molecule compound with a molecular weight of 102 Da. In the present study, a sandwich enzyme-linked immunosorbent assay (ELISA) for AOZ was developed. A novel derivatizing agent for AOZ was synthesized by linking 2-nitro-4-carboxybenzaldehyde and biotin with 1,6-hexanediol; the agent was added during sample pretreatment for AOZ derivatization with 92% yield. Sandwich ELISA for AOZ was developed by coating the ELISA plate with anti-AOZ monoclonal antibody and using horseradish peroxidase-labeled avidin or anti-biotin antibody as a secondary conjugate. From the perspective of application, the limit distances of the two epitopes under the double-antibody sandwich and antibody-avidin sandwich modes were 12 and 13 ?, respectively, and the ideal distances were uniformly ≥17 ?. The limit of detection of the double-antibody sandwich and antibody-avidin sandwich modes were 1.8 and 0.8 pg/mL (calculated using AOZ), respectively. Compared with competitive ELISA, the developed ELISA method achieved a 25-fold improvement in sensitivity. The average recovery rate and average relative standard deviation were 73%–85% and 9.0%, respectively.

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Development of a Detection method for Quaternary Ammonium Compounds in Food and Analysis of Their Contents in Commercial Food and Dietary Samples in Beijing

Yun XIE Wei-E Zhou Jing Zhang

FOOD SCIENCE 0, (): 0-0.

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An analytical method based on ultra-high-performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous detection of 9 commonly used quaternary ammonium compounds (QACs) in various food matrices including vegetables, fruits, and aquatic products. The enrichment and purification of QACs were achieved using an improved QuEChERS method, and the separation was performed on a BEH C18 column (100 × 3.0 mm, 1.7 μm) via gradient elution. QACs were detected with electrospray ionization mass spectrometry in positive ion mode. The limits of detection and quantification for 9 QACs in vegetables, fruits, and aquatic products were 0.2-5.0 μg/kg and 1.0-10.0 μg/kg, respectively. The method showed good linearity (r2 > 0.99) within the detection range of respective QACs. The spiked recoveries were 65.24-118.63% with relative standard deviations (RSDs) of 0.19-6.77%. The method was subsequently used to study the QACs residue in commercial food and dietary samples in Beijing. The detection rate of commercial food and dietary samples was 30.43% and 12%, respectively. The result of dietary intake risk assessment showed that the risk of QACs residue is acceptable.

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Geographical Origin Identification of Ningxia Lycium Barbarum Using Hyperspectral Imaging Technology

weidong yuan Hong-Zhe JIANG

FOOD SCIENCE 0, (): 0-0.

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Ningxia Lycium barbarum have unique organoleptic qualities and medicinal properties, and counterfeit Ningxia Lycium barbarum products are pervasive in the market. As a result, it is vital for producers, consumers and market economy to quickly identify the geographical origin of Lycium barbarum. This study aimed to develop a detection method based on hyperspectral imaging (400~1000 nm) combined with chemometrics to identify the diverse geographical origins of Lycium barbarum. Hyperspectral images of Lycium barbarum from five different production areas in Ningxia, Gansu, Inner Mongolia, Qinghai and Xinjiang were acquired, and spectral data was extracted from the region of interest based on threshold segmentation method. Multiple preprocessing methods were employed to eliminate the interference information from the spectra, and the performance showed that the discriminative model based on normalized reflectance spectrum (NR) exhibited better performance. Furthermore, the successive projections algorithm (SPA), competitive adaptive reweighted sampling (CARS), particle swarm optimization (PSO), iteratively retaining informative variables (IRIV), and CARS+IRIV were used to select characteristic wavelengths. The results showed that the simplified model, which utilized CARS+IRIV for wavelength selection, achieved the best performance. In models ranging from binary to quintuple classifications, the selected characteristic wavelengths accounted for only 15.6% to 27.7% of the full spectra. The correct classification rates obtained in the prediction set were 97.7%, 90.9%, 89.2%, and 87.1%, respectively. In addition, a confusion matrix was employed to visualize the optimal simplified classification model and intuitively distinguish the classification categories. Satisfactory sensitivity, specificity and Kappa coefficients were obtained in classifying Ningxia Lycium barbarum. The results illustrated that hyperspectral imaging technology combined with chemometric methods can effectively identify the geographical origin of Lycium barbarum and provide crucial technical support for the development of Lycium barbarum industry.

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Rapid Quantitative Authentication of Blended Vegetable Oil Quality by Raman Spectroscopy Coupled with a Selection Algorithm of Spectral Characteristic Intervals

WU Shengde, JIANG Xin, LI Aiqin, GUO Zhiming, ZHU Jiaji

FOOD SCIENCE 2024, 45 (6): 244-253. DOI: 10.7506/spkx1002-6630-20230531-291

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In this study, a method for the rapid quantitative determination of the content of high-value vegetable oil in blended edible vegetable oils (BEVO) was proposed based on Raman spectroscopy and a selection algorithm of spectral characteristic intervals. First, the particle swarm optimization (PSO) and grey wolf optimization (GWO) algorithms were combined to develop a hybrid intelligent optimization algorithm called PSOGWO. Second, the PSOGWO algorithm and the combined moving window (CMW) strategy were combined to develop a novel spectral characteristic interval selection algorithm named PSOGWO-CMW. Third, blends of corn oil (CO) and extra virgin olive oil (EVOO) at different ratios were prepared, and then their Raman spectra were acquired. Using the Raman spectra as input variables, partial least squares regression (PLSR), PSO-CMW, GWO-CMW, and PSOGWO-CMW models were developed to predict the content of EVOO, and their performance was comparatively studied. The results showed that the PSOGWO-CMW model had the best prediction performance. The results of the proposed method for the content of EVOO in CO-EVOO blends were not significantly different from those of gas chromatography-mass spectrometry. In conclusion, this method is rapid and accurate, and can be used for rapid and quantitative determination of the content of high-value vegetable oil in BEVO.

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Geographical Origin Identification of Lycium barbarum Fruit Using Hyperspectral Imaging Technology

YUAN Weidong, JIANG Hongzhe, YANG Shiyu, ZHANG Cong, ZHOU Yu, ZHOU Hongping

FOOD SCIENCE 2024, 45 (6): 254-260. DOI: 10.7506/spkx1002-6630-20230620-159

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This study aimed to develop a method based on hyperspectral imaging (400–1 000 nm) combined with chemometrics to identify the diverse geographical origins of Lycium barbarum fruit. Hyperspectral images of L. barbarum fruit from Ningxia, Gansu, Inner Mongolia, Qinghai and Xinjiang were acquired, and spectral data was extracted from the region of interest (ROI) by threshold segmentation method. Multiple preprocessing methods were employed to eliminate the interference information from the spectra, and the results showed that the discriminant model based on normalized reflectance spectrum (NR) exhibited better performance. Furthermore, the successive projection algorithm (SPA), competitive adaptive reweighted sampling (CARS), particle swarm optimization (PSO), iteratively retaining informative variables (IRIV), and CARS + IRIV were used to select characteristic wavelengths. The results showed that the simplified model based on the wavelengths selected by CARS + IRIV had the best performance. In the models ranging from binary to quintuple classifications, the selected characteristic wavelengths accounted for only 15.6% to 27.7% of the full spectra. The prediction accuracy was 97.7%, 90.9%, 89.2%, and 87.1%, respectively. In addition, a confusion matrix was employed to visualize the optimal simplified classification model in order to intuitively distinguish the classification categories. Satisfactory sensitivity, specificity and Kappa coefficients were obtained in classifying L. barbarum. The results illustrated that hyperspectral imaging technology combined with chemometric methods could effectively identify the geographical origin of L. barbarum and provide crucial technical support for the development of the L. barbarum industry.

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Development of a Detection Method for Quaternary Ammonium Compounds in Foods and Its Application to Commercial Foods and Dietary Samples in Beijing

XIE Yun, ZHOU Wei’e, XU Xiuli, ZHANG Jing, ZHANG Feng

FOOD SCIENCE 2024, 45 (6): 261-270. DOI: 10.7506/spkx1002-6630-20230613-105

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An analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous detection of nine commonly used quaternary ammonium compounds (QACs) in various food matrices including vegetables, fruits, and aquatic products. The enrichment and purification of QACs were achieved using an improved quick, easy, cheap, effective, rugged and safe (QuEChERS) method, and the separation was performed on a BEH C18 column (100 mm × 3.0 mm, 1.7 μm) with gradient elution. QACs were detected using an electrospray ionization source in the positive ion mode. The limits of detection and quantification for the nine QACs in vegetables, fruits, and aquatic products were 0.2–5.0 and 1.0–10.0 μg/kg, respectively, and good linearity was observed for all analytes within their respective concentration ranges (R2 > 0.99). The recoveries for spiked samples were in the range of 65.24%–118.63% with relative standard deviations (RSDs) of 0.19%–6.77%. When the developed method was applied to commercial foods and dietary samples in Beijing, detection rates of 30.43% and 12% were obtained, respectively. The dietary risk of QAC residues was acceptable.

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A Sandwich Immunosorbent Assay for 3-Amino-2-Oxazolidinone Following Derivatization

ZHANG Shiwei, WU Huiling, ZHOU Yingchun, WANG Bingzhi, YANG Xingxing, DU Yegang, TANG Lu, FENG Ronghu, GUO Jiping

FOOD SCIENCE 2024, 45 (6): 271-276. DOI: 10.7506/spkx1002-6630-20230509-079

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In the present study, a sandwich enzyme-linked immunosorbent assay (ELISA) for 3-amino-2-oxazolidnone (AOZ) was developed. A novel derivatizing agent for AOZ was synthesized by linking 2-nitro-4-carboxybenzaldehyde and biotin through 1,6-hexanediol. During the sample pretreatment, the agent was added for AOZ derivatization with an efficiency of 89%. The monoclonal antibody (McAb) against AOZ was coated on the microplate and horseradish peroxidase-labeled avidin or anti-biotin antibody was used as a secondary conjugate in the ELISA method. From a practical perspective, the limit distances between the two epitopes in the double-antibody sandwich and antibody-avidin sandwich modes were 12 and 13 Å, respectively, and the ideal distances were 16 and 17 Å, respectively. The detection limits of the double-antibody sandwich and antibody-avidin sandwich modes were 1.8 and 0.8 pg/mL for AOZ, respectively. Compared with competitive ELISA, a 25-fold improvement in the sensitivity of the developed ELISA method was achieved. The average recoveries and average relative standard deviations (RSDs) were 73%–85% and 9.0%, respectively.

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Determination of three sulfonamides residues in fish by graphene foam-based electrically enhanced Solid-phase Microextraction coupled with High Performance Liquid Chromatography

Xiao-mei CHEN

FOOD SCIENCE 0, (): 0-0.

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In order to improve the enrichment effect of sulfonamides (SAs) residues in fish, an electrically enhanced solid-phase microextraction (EE-SPME) method based on a nitrogen-doped three-dimensional graphene foam (NGF) functionalized monolithic column (Monolith@NGF, M@NGF), coupled with high-performance liquid chromatography (HPLC), was developed for the rapid and sensitive determination of sulfonamides (SAs) residues in fish. In this study, porous M@NGF was prepared on the surface of stainless steel wires by in situ polymerization using ionic liquids as functional monomers and NGF as a conductivity enhancer. An EE-SPME method was established for the extraction of sulfathiazole (ST), sulfadimethylpyrimidine (SM2), and sulfadimethoxypyrimidine (SMM) from fish, and the optimization of the adsorption time, adsorption voltage, pH value of sample solution, desorption time, desorption voltage, and the composition of desorption solution were performed. The results showed that the M@NGF-based EE-SPME method enriched ST, SM2 and SMM by multiples of 74, 58 and 64, respectively, and the adsorption equilibrium time was shortened to 35 min. The limits of detection (LODs) of this method were 1.78, 3.16 and 1.84 μg/kg, and the limits of quantification (LOQs) were all 5 μg/kg. The linear correlation coefficients (R2) of this method were all greater than 0.9990, and the recoveries were in the range of 79.2~110.1% with the relative standard deviations (RSDs) of 1.4~9.8% (n=5) in the linear range of 5~5000 μg/kg, respectively. This method solved the problems of low extraction efficiency and serious matrix interference of SAs residues in fish, and realized the rapid and sensitive detection of SAs residues in fish.

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Contamination in Fishery Products and Histamine Producing Ability of Morganella psychrotolerans, a Psychrotrophic Histamine-Producing Bacterium

LI Jin Di WANG Sheng-Jun CHEN Yan-Yan WU Chun-Sheng LI wang yueqi

FOOD SCIENCE 0, (): 0-0.

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Absract：Morganella psychrotolerans, as a psychrotolerant histamine-producing bacteria, can grow and produce histamine under low temperature conditions, resulting in the formation of high levels of histamine in cold-chain aquatic products, which can cause histamine food poisoning. However, studies on M. psychrotolerans in China are currently lacking. Therefore, this study aimed to investigate the presence of M. psychrotolerans in commercially available fish samples from Guangdong province. The results revealed a wide distribution of M. psychrotolerans with a contamination rate of 34%. The contamination rates for lean fish and white fish were 28% and 27.3% respectively. Specifically, mackerel samples had a contamination rate of 38.24%, while tuna samples had a rate of 29.41% among all positive samples. Sixteen strains of M. psychrotolerans were isolated from the positive samples. The capacity for histamine production by these isolates was examined, and it was found that all isolates produced histamine levels exceeding 1000 mg/L after 48 h incubation at 20 °C. Notably, isolate 1 showed histamine production that exceeded that of the type strain of M. psychrotolerans. Although isolate 1 and the type strain exhibited no significant differences in growth curve during incubation at varying temperatures (4 °C, 20 °C), their histamine production differed. The objective of this study was to assess M. psychrotolerans contamination in commercially available aquatic products in Guangdong province, as well as to examine the histamine production capacity of the isolates. The findings offer crucial theoretical support regarding the potential concern of histamine accumulation in the cold chain logistics of aquatic products.

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Determination of the Residues of Three Sulfonamides in Fish by Graphene Foam-Based Electro-Enhanced Solid-Phase Microextraction Coupled with High Performance Liquid Chromatography

SUN Ruixue, FANG Yuwen, CHEN Dongyan, CHEN Quansheng, CHEN Xiaomei

FOOD SCIENCE 2024, 45 (5): 265-274. DOI: 10.7506/spkx1002-6630-20230822-160

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A rapid and sensitive method for the determination of sulfonamide (SA) residues in fish was developed using electro-enhanced solid-phase microextraction (EE-SPME) based on nitrogen-doped three-dimensional graphene foam (NGF) functionalized monolithic column (monolith@NGF, M@NGF) combined with high performance liquid chromatography (HPLC). To improve the enrichment efficiency of SA residues in fish, porous M@NGF was prepared on the surface of stainless-steel wires by in situ polymerization using ionic liquids as the functional monomer and NGF as the conductivity enhancer. The EE-SPME method was applied for the extraction of sulfathiazole (ST), sulfamethazine (SM2), and sulfadimethoxypyrimidine (SMM) from fish. Adsorption time, agitation speed, adsorption voltage, ionic strength, the pH of sample solution, desorption time, desorption voltage, and the composition of desorption solution were optimized. The results showed that the M@NGF-based EE-SPME method enriched ST, SM2 and SMM by 74, 58 and 64 folds, respectively, and shortened the adsorption equilibrium time to 35 min. In the linear range of 5–5 000 μg/kg, the limits of detection (LODs) of this method were 1.78, 3.16 and 1.84 μg/kg for ST, SM2 and SMM, respectively, and the limits of quantification (LOQs) were 5 μg/kg for all analytes. Coefficients of determination (R2) for linear regression analysis of this method were all greater than 0.999 0, and the recoveries from spiked samples ranged from 79.2% to 110.1%, with relative standard deviations (RSDs) ranging from 1.4% to 9.8% (n = 5). This method solved the problems of low extraction efficiency and serious matrix interference of SA residues in fish, and allowed the rapid, sensitive detection of SA residues in fish.

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Contamination Status of Psychrotolerant Morganella psychrotolerans in Fish and Histamine-Producing Capacity of Its Isolates

LI Jin, WANG Di, CHEN Shengjun, WU Yanyan, LI Chunsheng, WANG Yueqi

FOOD SCIENCE 2024, 45 (5): 275-282. DOI: 10.7506/spkx1002-6630-20230830-222

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The contamination status of cold resistant Morganella psychrotolerans in commercially available aquatic products was investigated, and the generation of histamine by its isolates was explored. A total of 100 samples of commercially available fish from Guangdong province were surveyed. The results revealed a widespread distribution of M. psychrotolerans with a contamination rate of 34%. The contamination rates for red-fleshed and white-fleshed fish were 35.9% and 27.3%, respectively. Specifically, the mackerel samples had a contamination rate of 38.24%, and the tuna samples had a contamination rate of 29.41% among all positive samples. Sixteen strains of M. psychrotolerans were isolated from the positive samples, and all isolates produced histamine levels exceeding 1 000 mg/L after 48 h incubation at 20 ℃. Notably, isolate 1 showed higher histamine-producing capacity than the type strain. Although the two strains exhibited no significant differences in growth curves at varying temperatures (4 and 20 ℃), their histamine-producing capacities were different. After 10 days of culture at 4 ℃, histamine production was higher by isolate 1 than the type strain, while the opposite result was observed after 60 h of culture at 20 ℃. These findings offer crucial theoretical support for addressing the problem of histamine accumulation in cold chain aquatic products.

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Studies on detection of tasty nucleotide associations in low-salt potherb mustard and its changes during storage

Gui-Zhang GU Jin-Jie ZHANG

FOOD SCIENCE 0, (): 0-0.

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Abstract: In order to explore the changes of flavor nucleotide-related compounds in low-salt potherb mustard during storage and transportation, an effective detection method by High performance liquid chromatography (HPLC) was established. The changes of sensory quality and the content of flavor nucleotide-associated substances of low-salt potherb mustard during storage at (25±5) ℃ (J-25), (4±1) ℃ (J-4), (25±5) ℃ after sterilization (M-25) and (4±1) ℃ after sterilization (M-4) were analyzed. The results showed that 12 compounds related to flavor nucleotides were effectively separated within 33 min. Both sterilization and cold storage could inhibit the deterioration of sensory quality and flavor nucleotide-associated substances during storage, and sterilization combined with cold storage had the best effect. The contents of Adenosine triphosphate (ATP) and Inosine monophosphate (IMP) in group M-4 still maintained 29.7% and 66.4% of the initial values at 60 days, and the sensory quality was acceptable. The total amount of flavor nucleotide-associated compounds related to ATP in potherb mustard stored at (25±5) ℃ increased first and then decreased rapidly, and the sensory acceptance period of potherb mustard in group J-25 was only 9 days. Both sterilization and cold storage effectively inhibited the changes of flavor nucleotides (AMP, GMP, CMP, Uridine monophosphate (UMP)) related to nucleic acid metabolism in the potherb mustard during shelf life, and the total amount of these 4 kinds of flavor nucleotides in the group M-4 was still 4.30 mg/100 g at the end of storage. The metabolism of fermenting microorganisms in pickled potherb mustard and high temperature accelerated the deterioration of flavor nucleotide-related compounds during storage, and sterilization and cold storage were beneficial to the maintenance of flavor nucleotide-associated compounds, which provided certain theoretical support for the processing and storage of low-salt pickled potherb mustard.

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Authenticating Xinjiang Pishan Hong sheep based on multi-element fingerprint analysis

Chun-Hui ZHANG

FOOD SCIENCE 0, (): 0-0.

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The study explored a method based on multi-elements combined with multivariate analysis to identify and authenticate Xinjiang Pishan Hong sheep. A total of 36 Pishan Hong sheep and 36 Hu sheep were collected, and both longissimus thoracis (LTL) and semitendinosus muscles (ST) were selected to determine the 51 multi-elements by (Inductively coupled plasma mass spectrometry, ICP-MS). Results displayed that Hong sheep demonstrated characteristic elemental fingerprints in different muscle types compared to Hu sheep, which were mainly reflected by trace elements. The linear discriminant analysis results based on significant elements showed a good discrimination effect, which was mainly reflected in LTL muscle. The accuracies of sheep breeds and muscle types models were 100% and 99.29%, respectively. Besides, a total of 13 multi-elements (La, Zn, Cs, Sn, Ho, Fe, Rh, Co, Se, Te, Mo, Al and Sb) were used to identify Pishan Hong sheep, with Rh, Te, Ho being key elements to identify Pishan Hong lamb with higher VIP scores, which were the key elemental markers. These characteristic elements compositions were associated with the breed, muscles and geographical locations.

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Simultaneous Determination of 31 Foodborne Stimulant Drug Residues in Animal-derived Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with with pass-through solid phase extraction

LIU Chuan Yan-Qiu CHEN

FOOD SCIENCE 0, (): 0-0.

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Abstract: In order to solve the problems of different matrix effects and interference of foodborne doping testing in different animal-derived foods，a method was established for the determination of ten protein anabolic agents, eight glucocorticoids, and twelve diuretics in animal-derived foods by pass-through solid phase extraction -high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS). The sample was extracted with 5% formic acid in acetonitrile, and the extract was purified by pass-through solid phase extraction before being measured by liquid chromatography-tandem mass spectrometry. The internal standard method was used for quantification. The linear relationship of 30 foodborne stimulants was good within their respective concentration ranges. The average recoveries ranged from 67.5% to 114.3%, and the relative standard deviations were between 0.7% and 16.1% (n = 6). This method has the characteristics of high sensitivity, simple operation, large detection flux and high detection efficiency, improves the measurement accuracy under different complex substrates. It can meet the detection needs of 30 kinds of foodborne stimulants in animal-derived food for sports events.

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Determination of 176 PPCPs content in water samples by ultra-performance liquid chromatography-tandem mass spectrometry

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FOOD SCIENCE 0, (): 0-0.

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Abstract: A method for simultaneous determination of 176 PPCPs (Pharmaceuticals and Personal Care Products) in water samples was established by combining solid-phase extraction (SPE) with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS). The water samples were adjusted to pH 7, and then subjected to enrichment and purification by Cleanert PEP solid-phase extraction column. After elution, the DMSO-assisted concentration was used for the wash solution, and the separation was carried out on HSS T3 column (2.1 mm × 150 mm, 1.8 μm) using methanol-0.1% formic acid water (containing 0.2 mMol ammonium acetate) as the mobile phase. The determination was performed in positive and negative ion switching modes with multiple reactions monitoring (MRM). Methodological validation results showed that the linear relationship of 176 PPCPs was good in the range of 5-200 ng/mL, with a correlation coefficient higher than 0.99. The quantitative limit of the method for 176 PPCPs was 0.1 ng/mL. In the blank water samples, the average recovery rate of 176 compounds was between 68.0% and 126.7% at three spiked levels (0.1 ng/mL, 0.4 ng/mL, and 1.0 ng/mL), with an RSD between 1.1% and 10.3% (n=6). The established method is simple, rapid, highly reproducible, and sensitive, and can meet the high-throughput detection requirements for 176 PPCPs in water samples.

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Simultaneous Determination of 30 Foodborne Stimulant Drug Residues in Animal-Derived Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-Through Solid Phase Extraction

LIU Chuan, LI Jiajia, WU Xueying, CHEN Yanqiu, SHI Peiyu, SONG Juan, DAI Qin

FOOD SCIENCE 2024, 45 (4): 289-299. DOI: 10.7506/spkx1002-6630-20230427-268

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In order to solve the problems of the detection of various foodborne stimulants in different animal-derived foods such as significant differences in matrix effects and many types of interference, a method was established for the determination of 10 protein anabolic agents, 8 glucocorticoids, and 12 diuretics in animal-derived foods by pass-through solid phase extraction (SPE) and ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with 5% formic acid in acetonitrile, and the extract was purified by pass-through solid phase extraction before being analyzed by UPLC-MS/MS. The internal standard method was used for quantification. The results showed that good linearity was observed for all analytes within their respective concentration ranges. The average recoveries ranged from 67.5% to 114.3% with relative standard deviations (RSDs) between 0.7% and 16.1% (n = 6). This method is characterized by high sensitivity, simple operation, high throughput and high detection efficiency, which improves the measurement accuracy of different complex matrices and can meet the need for the detection of the 30 foodborne stimulants in animal-derived foods used in sports events.

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Authentication of Xinjiang Pishan Hong Sheep Meat Based on Multi-element Fingerprinting

ZHAO Laiyu, ZHANG Hongru, WANG Jing, ZHANG Chunhui

FOOD SCIENCE 2024, 45 (4): 300-306. DOI: 10.7506/spkx1002-6630-20230509-077

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The study explored a method based on multi-elements combined with multivariate analysis to authenticate Xinjiang Pishan Hong sheep meat. A total of 36 Pishan Hong sheep and 36 Hu sheep were collected and slaughtered. Semitendinosus and longissimus dorsi muscles were excised from each carcass for analysis of 51 mineral elements by inductively coupled plasma mass spectrometry (ICP-MS). Results indicated that the mineral elements, especially rare elements, in Xinjiang Pishan Hong sheep meat had distinctive fingerprint characteristics. The linear discriminant analysis (LDA) model built based on the mineral element data showed good discriminant performance for Xinjiang Pishan Hong sheep meat, especially longissimus dorsi with an accuracy of 100% and 99.29% for breed and muscle, respectively. Besides, La, Zn, Cs, Sn, Ho, Fe, Rh, Co, Se, Te, Mo, Al and Sb could be used as the major mineral elements to identify Pishan Hong sheep meat. Among them, Rh, Te and Ho had the highest variable importance in the projection (VIP) scores, and were found only in Pishan Hong sheep meat, thus being the key mineral markers for identifying Pishan Hong sheep meat. The accumulation of characteristic elements was related to regional characteristics.

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Determination of the Concentrations of 176 Pharmaceutical and Personal Care Products in Drinking Water Samples by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

WU Shaoming, LIU Wenjing, DAI Ming, HE Menghang, CHEN Yankai, WANG Zheng, ZHAN Chongqing, OUYANG Liqun

FOOD SCIENCE 2024, 45 (4): 307-314. DOI: 10.7506/spkx1002-6630-20230530-282

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A method for simultaneous determination of 176 pharmaceuticals and personal care products (PPCPs) in drinking water samples was established by combining solid-phase extraction (SPE) with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The water samples were adjusted to pH 7, and then subjected to enrichment and purification using a Cleanert PEP SPE column. After concentration of the eluate with dimethyl sulfoxide (DMSO), the chromatographic separation was carried out on an HSS T3 column (2.1 mm × 150 mm, 1.8 μm) using methanol-0.1% formic acid water (containing 0.2 mmol ammonium acetate) as the mobile phase. The detection was performed in positive and negative ionization switching modes with multiple reaction monitoring (MRM). Methodological validation results showed that good linearity for the 176 PPCPs was achieved in the concentration range of 5–200 ng/mL, with a correlation coefficient higher than 0.99. The limit of quantitation (LOQ) of the method for all the PPCPs was 0.1 ng/mL. The average recoveries of spiked blank samples at three levels (0.1, 0.4 and 1.0 ng/mL) were between 68.0% and 126.7%, with relative standard deviation (RSD) between 1.1% and 10.3% (n = 6). In conclusion, the method established in this study is simple, rapid, reproducible, and highly sensitive, and can meet the requirements of the high-throughput detection of the 176 PPCPs in drinking water sources.

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