Determination of 60 Food-Borne Stimulant Drug Residues in Animal-Derived Foods by Solid-Phase Extraction Purification and Ultra-High-Performance Liquid Chromatography-Quadrupole/Orbitrap High-Resolution Mass Spectrometry

He, Liangna; Li, Qiang; Ma, Junmei; Cao, Meirong; Fan, Lixin; Ren, Xiaowei; Shi, Guohua; Zhang, Yan

doi:https://doi.org/10.1155/2024/3859819

Journal of Food Quality

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Abstract Introduction Materials and Methods Results and Discussion Conclusions Data Availability Conflicts of Interest Authors’ Contributions Acknowledgments Supplementary Materials References Copyright Related Articles

Research Article | Open Access

Volume 2024 | Article ID 3859819 | https://doi.org/10.1155/2024/3859819

Determination of 60 Food-Borne Stimulant Drug Residues in Animal-Derived Foods by Solid-Phase Extraction Purification and Ultra-High-Performance Liquid Chromatography-Quadrupole/Orbitrap High-Resolution Mass Spectrometry

Liangna He,¹Qiang Li,¹Junmei Ma,¹Meirong Cao,¹Lixin Fan,¹Xiaowei Ren,¹Guohua Shi,¹and Yan Zhang¹

Academic Editor: Timothy Omara

Received04 Oct 2023

Revised03 Jan 2024

Accepted18 Jan 2024

Published01 Feb 2024

Abstract

A method for the rapid screening and confirmation of 60 food-borne stimulants in animal-derived foods was developed using the ultra-high-performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry (UPLC-Q/Orbitrap HRMS). After enzymatic hydrolysis at 37°C for 16 h, the samples were extracted with acetonitrile solution. The extraction solution was purified by PRiME HLB pass-through solid-phase extraction cartridge and redissolved by nitrogen blowing. The target compounds of reconstitution fluid were separated by Hypersil GOLD™ VANQUISH column (2.1 mm × 100 mm, 1.9 μm). The raw data were collected for the target compounds in Full Scan-ddMS² mode, and then the Quan Browser module under Xcalibur software can be used to analyze the quantitative results of the samples. The combination of Tracefinder and mzVault software can realize the qualitative screening and confirmation of the samples. The results showed that the relative deviation of the exact mass of the 60 food-borne stimulants was less than 5.0 × 10⁻⁶, which had a good linear relationship in the corresponding concentration, and the correlation coefficient () was greater than 0.9966. The detection limit ranged from 0.05 to 0.5 μg/kg. The quantification limit ranged from 0.1 to 1 μg/kg. The method recoveries ranged from 70.2% to 111.9% with relative standard deviations of 0.05% to 9.00% (n = 6). The method is easy to operate, covers a wide range of targets, and has high efficiency and accuracy. It is suitable for rapid screening and confirmation of various food-derived stimulants in animal-derived foods and provides assistance for food safety in the major events.

1. Introduction

Animal-derived food refers to the products derived from animals and available for human consumption, including fresh meat, frozen meat and their products, eggs, and milk and meat products, which are the main sources of energy and protein intake for human beings. In order to meet the demand of human beings for animal-derived food, the scale of animal husbandry and aquaculture is expanding gradually. At the same time, in order to maximize economic benefits, some farmers illegally use prohibited drugs in the breeding process, resulting in animal-derived food containing a large amount of drug residues, which threatens the interests of consumers [1, 2]. In addition, the stimulant drug residues in animal-derived foods continue to harm human health, but also damage the fairness of competitive sports. For example, the doping problems emerge endlessly during the Olympic Games [3]. In order to eradicate this problem, ensure the fair competition of athletes and realize the original intention of successfully holding large-scale competitions, it is imperative to establish a technical means of simultaneous screening and quantification of various food-borne doping agents.

At present, the detection and analysis of stimulant drug residues in animal-derived foods includes enzyme-linked immunosorbent assay (ELISA) [4, 5], gas chromatography (GC) [6], gas chromatography-tandem mass spectrometry (GC-MS/MS) [7–9], liquid chromatography (LC) [10–12], liquid chromatography-tandem mass spectrometry (LC-MS/MS) [13–24], and liquid chromatography-high resolution mass spectrometry (LC-HRMS) [25–29]. Antibodies used in ELISA are produced by different manufacturers, and the quality is difficult to guarantee, resulting in differences between the results, and the cross-reaction phenomenon of immunology makes the test results prone to false positive. The pretreatment used by GC and GC-MS/MS is complicated, and its detection limit is high, so it is difficult to achieve high-sensitivity detection and analysis. LC performs qualitative and quantitative analysis only by retention time, so the number of compounds analyzed within a certain time window is limited. Compared with LC, LC-MS/MS can obtain information such as the ion ratio of compounds and realize the simultaneous analysis and detection of multiple compounds, it cannot obtain abundant information of product ion fragments, and the accurate of first-order mass obtained by LC-MS/MS is relatively low, which makes it impossible to achieve high-throughput screening analysis. LC-HRMS can obtain the characteristic secondary fragment ion information of the compound, and its mass accuracy can reach ppm level, which has higher resolution, and high-throughput qualitative and quantitative analysis can be achieved in combination with the secondary spectral library information.

The research reports on food-borne stimulants mainly focus on β2 adrenoceptor agonists or specific types of stimulants, and there are few reports on the simultaneous detection of multiple stimulants. Feng et al. used ultra-high-performance liquid chromatography-tandem mass spectrometer to determine 44 kinds of food-borne stimulants and 6 kinds of progesterone in livestock and poultry meat [30]. This method measured a variety of food-borne stimulants and covered a wide range, and they could not obtain information such as fragment ion and isotope ratio, and had weak qualitative ability for complex samples. Yan et al. used high-throughput analytical platform to screen 39 glucocorticoids in animal-derived food [27]. In this experiment, UPLC-Q/Orbitrap HRMS with ultrahigh resolution and high selectivity was used as the detector of food-borne stimulants in animal-derived foods. PRiME HLB solid-phase extraction column was used to eliminate impurities in the samples. A secondary spectrum library of 60 food-borne stimulants and 12 kinds of diuretics, 18 kinds of protein anabolic agents, 9 kinds of glucocorticoids, 18 kinds of β2 adrenoceptor agonists, 3 kinds of β-receptor antagonists for simultaneous screening and quantification of animal food was analyzed. This method can further improve the qualitative credibility, ensures the accuracy of positive samples, and can further avoid the occurrence of athletes taking food-borne stimulants by mistake, and provides technical guarantee for the screening of food-borne stimulants in large-scale competitions.

2. Materials and Methods

2.1. Apparatus, Chemicals, and Reagents

Vanquish Flex + Orbitrap Exploris 480 ultra-high-performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (Thermo Fisher Scientific, USA) was used. Instrument control and data acquisition were realized by Thermo Scientific Xcalibur. Data screening analysis was realized by the combination of TraceFinder and mzVault software. The content of detected residues was calculated by Thermo Xcalibur Quan Browser. The high-speed refrigerated centrifuge (CR22N, HITACHI, Germany), the ultrasonic cleaner (Elmasonic P300H, Elma, Germany), vortex mixer (Vortex Genius 3, IKA, Germany), and nitrogen blower (Organomation, USA) was used.

Clenbuterol, salbutamol, ractopamine, terbutaline, fenoterol, tulobuterol, penbutolol, cimaterol, salmeterol, atenolol, metoprolol, clenproperol, demethyl coclaurine, tretoquinol, propanolol, bromoclenbuterol, formoterol, brombuterol, meprednisone, prednisolone, methylprednisolone, dexamethasone, betamethasone, beclomethasone, fludrocortisone, hydrocortisone, cortisone, zilpaterol, stanozolol, trenbolone, metandienone, 17-methyltestosterone, testosterone, nandrolone, testosterone propionate, nandrolone 17-propionate, boldenone, nandrolone phenylpropionate, dehydroepiandrosterone, zeranol, beta-zearalanol, alpha-zearalenol, beta-zearalenol, zearalanone, zearalenone, acetazolamide, canrenone, chlortalidone, furosemide, spironolactone, bendroflumethiazide, chlorothiazide, hydrochlorothiazide, triamterene, 4-amino-6-chlorobenzene-1,3-disulfonamide, bumetanide, torasemide, acebutolol, and celipolol (purity ≥95%) were supplied from Dr. Ehrenstorfer (Augsburg, Germany). All the samples used in this experiment were purchased from Qiaoxi vegetable wholesale market in Shijiazhuang.

Methanol, acetonitrile, formic acid, and ammonium acetate were of HPLC grade and were purchased from Merck (Darmstadt, Germany). Waters Oasis PRiME HLB solid-phase extraction column (200 mg, 6 cc) was purchased from Waters (USA). Water was purified using a Milli-Q-System (Millipore, Guyancourt, France). β-glucuronidase/arylsulfatase (contains β-glucuronidase 111000 U/mL and arylsulfatase 1079 U/mL) was purchased from Sigma (USA).

2.2. Preparation of Standard Solution

Weigh an appropriate amount of standards, respectively, into a 100 mL volumetric flask, dissolved it with methanol and make up to the mark (triamterene should be dissolved in formic acid first, and then make up to the mark with methanol). The standard reserve solution with mass concentration of 100 μg/mL, store it at −20°C and valid for 6 months. The standard reserve solution was pipetted to a 100 mL volumetric flask, respectively, and dissolving in methanol to scale. The concentration of ractopamine, fenoterol, tulobuterol, salmeterol, metoprolol, propanolol, trenbolone, and nandrolone phenylpropionate in the obtained mixed standard intermediate solution is 1 μg/mL, the concentration of clenbuterol, salbutamol, terbutaline, penbutolol, cimaterol, atenolol, clenproperol, demethyl coclaurine, tretoquinol, meprednisone, prednisolone, methylprednisolone, dexamethasone, betamethasone, beclomethasone, fludrocortisone, hydrocortisone, cortisone, zilpaterol, stanozolol, metandienone, 17-methyltestosterone, testosterone, nandrolone, testosterone propionate, nandrolone 17-propionate, boldenone, dehydroepiandrosterone, zeranol, beta-zearalanol, alpha-zearalenol, beta-zearalenol, zearalanone, zearalenone, acebutolol, bromoclenbuterol, celipolol, formoterol, brombuterol, and nebivolol is 2 μg/mL, and the concentration of acetazolamide, canrenone, chlortalidone, furosemide, spironolactone, bendroflumethiazide, chlorothiazide, hydrochlorothiazide, triamterene, 4-amino-6-chlorobenzene-1,3-disulfonamide, bumetanide, and torasemide is 10 μg/mL. The solution was stored at −20°C and valid for 3 months. The 14 kinds of internal standard materials were weighed and dissolved in 10 mL volumetric flask with methanol, and the volume was fixed to the scale. The mixed standard reserve solution with mass concentration of 100 μg/mL was obtained. It was stored at −20°C and valid for 6 months.

2.3. Sample Preparation

5 g (milk, egg, beef, mutton, and pork) of homogenized sample was weighed and transferred to a 50 mL plastic centrifuge tube, then spiking of 10 μL of 1 μg/mL internal standard solution, 20 mL of 0.2 mol/L acetic acid ammonium buffer (pH = 5.2 ± 0.1), and 50 μL of β-glucuronidase/arylsulfatase, vortexed for 1 min to mix. The sample was placed in a water bath shaker at 37 ± 1°C and shaked for enzymatic hydrolysis 16 h. The enzymolysis sample solution was cooled to room temperature, centrifuged at 10000 r/min for 5 min, and then supernatant A was removed. 10 mL acetonitrile solution was added to supernatant A, then 8 g sodium chloride was added, and the extraction was conducted by shaking for 10 min. The mixed solution was centrifuged at 10000 r/min for 5 min, and supernatant B was taken. 10 mL acetonitrile solution was added to supernatant A and was extracted by shaking for 10 min. The mixed solution was centrifuged at 10000 r/min for 5 min, and supernatant C was taken. Supernatant B and supernatant C were combined and passed through the PRiME HLB solid-phase extraction column with a flow rate of 1 drop/s. The outflow was collected and blown to near dry at 40°C with nitrogen. 1 mL of initial mobile phase was added and mixed by vortex. The complex solution was filtered by 0.22 μm nylon membrane and was determined. The animal food without the target compound was pretreated according to the above experimental method, and the blank matrix solution was obtained, which was used for the preparation of the standard curve except the internal standard material.

2.4. Chromatographic Conditions

The chromatographic separation was performed on a Hypersil GOLD™ VANQUISH column (2.1 mm × 100 mm, 1.9 μm, Thermo Fisher Scientific, USA). The injection volume was 5 μL. The flow rate was 0.3 mL/min. Aqueous solution containing 0.1% (v/v) formic acid (phase A) and 50% methanol-acetonitrile solution (phase B) were used as mobile phase. The consecutive program was as follows: 0–3.00 min, 2% to 30% B; 3.00–15.00 min, 30% to 50% B; 15.00–18.00 min, 50% to 95% B; 18.00–20.00 min, 95% B; 20.00–20.10 min, 95% to 2% B; and 20.10–22.00 min, 2% B.

2.5. Mass Spectrometry Conditions

The MS analysis was performed using an ESI source in positive/negative ionization mode. The optimized parameters of ion source were as follows: the positive ion/negative ion was +3500/−3000 V, the ion transfer tube temp was 320°C, the vaporizer temp was 400°C, the sheath gas was 45 Arb, the aux gas was 10 Arb, and the sweep gas was 1 Arb. MS conditions were as follows: scan type was Full Scan-ddMS², scan range was 150–800 m/z, the duration was 22 min, the collision energy mode was stepped, the collision energy type was normalized, HCD collision energies was 30 V, 50 V, and 70 V, Full Scan orbitrap FWHM was 60000, and MS² orbitrap FWHM was 30000.

2.6. Establishment of Database

Under the instrument conditions given in Sections 2.4 and 2.5, the 60 kinds of food-borne stimulants name, molecular formula, and the way of ionization was inputted instrument after acquisition method. The data of doping were collected, such as the retention time. Then, the time window was set to 1 min, realize the precise analysis of the specific compounds. The detailed parameter information of 60 compounds is shown in Table 1. This study was confirmed by the matching degree of a high-resolution precursor ion and the secondary spectrum, and the mass deviation of both parent ion and fragment ion was less than 5 ppm. In the ddMS² mode of Vanquish Flex + Orbitrap Exploris 480, when a specific target compound responds within the set retention time window, it is automatically triggered to collect and superimpose at different collision energies (30 V, 50 V, and 70 V) to generate secondary fragment spectra. In the database Library module of Thermo mzVault software, import raw data to create a secondary spectrum library including 60 food-borne stimulants, the MS² spectra of the 60 food-borne stimulants are shown in Supplementary Figure 1.

3. Results and Discussion

3.1. Optimization of Liquid Chromatography Conditions

Under the same mobile phase, 60 target compounds were investigated on ACQUITY UPLC® HSS C18 column (2.1 mm × 100 mm, 1.8 µm), Waters Acquity UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 µm), Kinetex C18 column (2.1 mm × 100 mm, 2.6 μm), and Hypersil GOLD™ VANQUISH column (2.1 mm × 100 mm, 1.9 μm) separation effect and peak shape. The experiment found that Hypersil GOLD™ VANQUISH column can convert five groups of isomers: dexamethasone and betamethasone with parent ion (m/z) of 393.21, spironolactone and canrenone with parent ion (m/z) of 341.21, cortisone and prednisolone with a parent ion (m/z) of 361.20 and α-zearyl alcohol and β-zearyl alcohol with a parent ion (m/z) of 321.17, zearalenol, β-zearalenol, and zearalenone with a parent ion (m/z) of 319.155 were effectively separated. Therefore, Hypersil GOLD™ VANQUISH column (2.1 mm × 100 mm, 1.9 μm) was selected as the chromatographic column for this method. In this study, the effects of acetonitrile-water, methanol-water, 0.1% acetonitrile-0.1% formic water, 0.1% methanol-0.1% formic water, and 50% methanol-acetonitrile-0.1% formic water as mobile phases were investigated. The results showed that when acetonitrile-water and methanol-water were mobile phases, the peak pattern of each component was poor and the positive ion response was low. The negative ion response is low when the mobile phase is 0.1% acetonitrile-0.1% formic acid water and 0.1% methanol-0.1% formic acid water. When 50% methanol-acetonitrile-0.1% formic acid water was used as mobile phase, the peak pattern of each component was improved obviously, and the response value was the best.

3.2. Optimization of Mass Spectrometry Parameters

Vanquish Flex + Orbitrap Exploris 480 dedicated low-flow ESI ion source for systematic calibration. At the same time, during the data acquisition process, Easy-IC was set to on in the process of data collection, and the Easy-IC source was activated to generate fluoranthene ion, which is injected into C-trap (2 ms) for internal standard correction of the system. After the correction is passed, the ion of the object to be measured will be introduced into the mass spectrometry system for detection and analysis. The Vanquish Flex + Orbitrap Exploris 480 uses an internal calibration source to calibrate the positive and negative ion modes in real time, ensuring accurate and stable mass numbers for the duration of the mass spectrum. Parameters such as Vaporizer Temp, Sweep Gas, CUR, and HCD Collision Energy were optimized using Vanquish Flex + Orbitrap Exploris 480. Different information on the secondary fragment ions of the target compound was found with different HCD Collision Energy values entered. It was found that the HCD Collision Energy input 30 V, 50 V, and 70 V in the Stepped Mode of Collision Energy Mode, and the obtained secondary spectrum is the fragment ion adduct generated by the collision of the target compound at three energies, and the fragment ion information is more abundant. In Full Scan-ddMS² mode, the information of primary parent ions and secondary fragment ions of the target compound was collected simultaneously, and ion chromatograms were extracted according to their molecular ion peaks [M + H]⁺ or [M − H]⁻ theoretical accurate mass number (Supplementary Figure 2). The relative deviations of the accurate mass numbers of the 60 food-borne stimulants are all less than 5.0 × 10⁻⁶, as shown in Table 1, in line with the LC/MS regulations of the European Union [31], which can be used for qualitative and quantitative analysis of the target compounds.

3.3. Optimization of Extraction Solvents

In this experiment, the recoveries of 60 target compounds were investigated by ethyl acetate, methanol, and acetonitrile, respectively, as shown in Figure 1. The results showed that the average recoveries of 60 target compounds after ethyl acetate extraction ranged from 55% to 125%. In the process of nitrogen blowing or rotary evaporation, white lipids were gradually precipitated from the methanol extract. The average recovery of acetonitrile was between 70% and 110%, so acetonitrile was used as the extraction solvent in this experiment.

3.4. Optimization of Purification Methods

The matrix of animal-derived food is relatively complex, and it contains a large amount of protein, fat, and other substances, which will interfere with the accuracy of detection results. MCX solid-phase extraction column was usually used purification method of β-stimulants. However, the recovery rate of β-receptor antagonists is poor [32]. Therefore, HLB and PRiME HLB solid-phase extraction columns can also remove impurities in the sample and achieve purification effect, which were, respectively, used in this experiment to purify the extracted liquid, as shown in Figure 2. The results showed that the recovery rate of target compounds after purification by PRiME HLB solid-phase extraction column were higher than that of HLB. PRiME HLB can achieve rapid purification effect without activation, elution, and other tedious processes, which is suitable for the detection of food-borne stimulants in a large number of animal-derived foods.

3.5. Matrix Effects

In this study, the ratio of slopes of the standard curves drawn by matrix and solvent was used to evaluate the influence of matrix effect (ME, , is the slope of the blank matrix standard curve, and is the slope of the methanol standard curve) on the experimental results. When the ratio was in the range of 0.85∼1.15, the influence of ME on the experimental results was considered to be negligible [33, 34]. In this experiment, beef was used as the matrix to investigate the matrix effect, and the results are shown in Table 2. 24 kinds of compounds showed no significant matrix effect, and the signal intensity of the other compounds was significantly inhibited or enhanced. In order to eliminate the influence of matrix effect, blank matrix extract was used to match the standard curve.

3.6. Linearity and Sensitivity

Accurately absorb 60 kinds of food-borne stimulants mixed standard intermediate solutions, and use blank matrix extract to prepare a series of standard working solutions. The ratio of the parent ion peak area of the compound to be measured and the concentration of the corresponding standard solution (ng/mL) was used as the vertical coordinate to draw the standard curve. The limits of detection (LOD) and quantitation (LOQ) of the method were determined according to the blank matrix addition method, with S/N = 3 as LOD and S/N = 10 as LOQ. As shown in Table 2, the 60 food-borne stimulants had a good linear relationship in the corresponding concentration, the correlation coefficient () was more than 0.9966, the LOD was 0.05–0.5 μg/kg, and the LOQ was 0.1–1 μg/kg.

3.7. Recovery and Precision

60 kinds of food-borne stimulants standard substances were added to blank milk, egg, beef, mutton, and pork matrix for the spiked recovery experiment. Three concentration levels were added in total, and each concentration level was tested for 6 times. The results are shown in Table 3. The results showed that the average recoveries of milk, egg, beef, mutton, and pork ranged from 72.8% to 111.9%, 72.0% to 111.8%, 70.2% to 110.8%, 73.4% to 111.7%, and 75.4% to 111.0%, respectively, and the relative standard deviation (RSD) ranged from 0.05% to 8.97%, 0.05% to 8.88%, 0.05% to 8.94%, 0.05% to 8.88%, and 0.05% to 9.00%, respectively.

3.8. Sample Analysis

In order to investigate the applicability of the method, 30 milk samples, 30 egg samples, 50 beef samples, 50 mutton samples, and 50 pork samples randomly selected in the market were tested. The results are shown in Table 4. In addition, we validated the quantitative analysis quality control samples of clenbuterol, salbutamol, and ractopamine in beef from the Chinese Academy of Inspection and Quarantine (certificate number: 303RG04081), and the results showed that the detection values of the three substances were all within the range of characteristic values, which proved that the detection method was effective.

4. Conclusions

In this study, the PRiME HLB solid-phase extraction column purification was combined with the UPLC-Q/Orbitrap HRMS to realize the rapid detection of 60 food-borne stimulants in animal-derived foods. The purification process of this method requires no steps such as activation, balancing, and leaching, which simplifies the operation procedure of pretreatment. Data collection was carried out in Full Scan-ddMS² mode, quantitative analysis was performed based on the ion peak area of first-order mass, and information such as retention time, secondary fragment ion information, and accurate mass was used to establish information including diuretics, protein anabolic agents, glucocorticoids, β2 adrenoceptor agonists, β-receptor antagonists, and other five types of 60 kinds of food-borne doping secondary spectrum library. Unknown samples can be screened and confirmed without reliance on standard substances. The method has the advantages of simple and rapid pretreatment, wide coverage of doping types, strong applicability, and high accuracy of results. It avoids the occurrence of accidental intake of food-borne doping by athletes, and maintains the fairness and justice of competitive sports.

Data Availability

The data used to support the findings of this study are included within the article.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Authors’ Contributions

YZ and GH conceived and designed the experiments. LH, QL, JM, and MC performed the experiments. LF and XR analyzed the data; LH and QL wrote the original draft. All authors have read and approved the manuscript. Liangna He and Qiang Li have contributed equally to this work. Liangna He and Qiang Li share first authorship.

Acknowledgments

This work was supported by the Science and Technology Project of Hebei Province (21475501D) and the High-Level Talents Funding Project of Hebei Provincial (A202001058).

Supplementary Materials

Supplementary Figure 1: MS² spectra of the 60 food-borne stimulants. Supplementary Figure 2: extracted ion chromatograms of the 60 food-borne stimulants. (Supplementary Materials)

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Copyright © 2024 Liangna He et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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