PMID- 35080161 OWN - NLM STAT- MEDLINE DCOM- 20220127 LR - 20220915 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 40 IP - 2 DP - 2022 Feb 8 TI - [Determination of nine food-borne stimulant drug residues in pork, egg, and milk by ultra-performance liquid chromatography-tandem mass spectrometry]. PG - 148-155 LID - 10.3724/SP.J.1123.2021.04005 [doi] AB - beta-Agonists, beta-blockers, and protein assimilators are classified as stimulant drugs. Their illegal use during animal feeding and slaughtering leads to food-borne stimulant drug residues, which are harmful to human health. At present, methods for the detection of beta-agonists and protein assimilators are prevalent, but those for the detection of beta-blockers are rare. There is no national standard for the detection of beta-blockers in food products of animal origin. A method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of nine food-borne stimulant drug residues, including beta-agonists, beta-blockers, and protein assimilators, in pork, egg, and milk. The optimal extraction conditions for this method were as follows: The samples were hydrolyzed with beta-glucuronidase/aryl sulfate esterase in pH 5.2 ammonium acetate buffer. Enzymatic hydrolysis was carried out in a constant-temperature (37 ℃) water bath oscillator for 16 h. The enzymolyzed samples were cooled to room temperature and then extracted with acetonitrile, which was adjusted to pH 9.5 with NaOH solution. After extraction and homogeneous mixing, the extract was added to a salt package for salting out stratification. The clear supernatant was cleaned up using an enhanced lipid removal tube (EMR-lipid), which was pre-activated by water. Then, anhydrous magnesium sulfate was added to ensure dehydration of the extract and concentrated to near dryness under nitrogen flow. The residue was dissolved in 1 mL acetonitrile-0.1% formic acid aqueous solution (1ratio9, v/v). Separation was performed on an ACQUITY UPLC HSS T3 column (100 mmx2.1 mm, 1.8 mum) with gradient elution using methanol-0.1% formic acid aqueous solution as the mobile phase. The analytes were detected in the multiple reaction monitoring (MRM) mode after being ionized by an electrospray positive ion (ESI(+)). Quantitative analysis was performed by the internal standard method using matrix-matched calibration curves. The effects of the extraction solvent and pH on the extraction efficiency during pretreatment were optimized. The influence factors of different types of chromatographic column, mobile phase and dissolved solution in the process of instrumental analysis were discussed in detail. Under the optimal conditions, the method showed good linearity in the range of 0.5 to 20 mug/L, with correlation coefficients (r(2)) greater than 0.99. The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.3-0.6 mug/kg and 1.0-2.0 mug/kg, respectively. The average recoveries of all the compounds ranged from 65.2% to 117.0% with relative standard deviations (RSDs) in range of 1.3%-14.4% at spiked levels of 1, 2, and 5 times the LOQs. The established method was used to determine the quality of animal-origin foods such as pork, eggs, and milk purchased from the market. The nine stimulant drug residues were not detected in these food samples. The analytical method is rapid, sensitive, accurate, and stable. It can be used for the determination of the nine food-borne stimulant drugs residue in pork, egg, and milk. FAU - Liu, Xuezhi AU - Liu X AD - Chinese Academy of Inspection and Quarantine Comprehensive Test Center, Beijing 100123, China. FAU - Zhao, Yinglian AU - Zhao Y AD - Chinese Academy of Inspection and Quarantine Comprehensive Test Center, Beijing 100123, China. FAU - Ma, Yue AU - Ma Y AD - China Inspection Branch (Beijing) Test Technology Co., Ltd., Beijing 100176, China. FAU - Dong, Shishi AU - Dong S AD - Chinese Academy of Inspection and Quarantine Comprehensive Test Center, Beijing 100123, China. FAU - Wang, Bin AU - Wang B AD - Chinese Academy of Inspection and Quarantine Comprehensive Test Center, Beijing 100123, China. FAU - Zhang, Yang AU - Zhang Y AD - China Inspection Branch (Beijing) Test Technology Co., Ltd., Beijing 100176, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 SB - IM MH - Animals MH - Chromatography, High Pressure Liquid MH - Chromatography, Liquid MH - *Drug Residues/analysis MH - Food Contamination/analysis MH - Humans MH - Milk MH - *Pork Meat MH - *Red Meat MH - Solid Phase Extraction MH - Swine MH - Tandem Mass Spectrometry PMC - PMC9404034 OTO - NOTNLM OT - egg OT - food-borne stimulant drug OT - milk OT - pork OT - residues OT - ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) EDAT- 2022/01/27 06:00 MHDA- 2022/01/28 06:00 PMCR- 2022/02/08 CRDT- 2022/01/26 05:34 PHST- 2022/01/26 05:34 [entrez] PHST- 2022/01/27 06:00 [pubmed] PHST- 2022/01/28 06:00 [medline] PHST- 2022/02/08 00:00 [pmc-release] AID - 1000-8713-40-2-148 [pii] AID - 10.3724/SP.J.1123.2021.04005 [doi] PST - ppublish SO - Se Pu. 2022 Feb 8;40(2):148-155. doi: 10.3724/SP.J.1123.2021.04005.