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  • Title: [Simultaneous determination of 40 plant growth regulators, fungicides, insecticides, and antibiotics in bean sprouts by QuEChERS-high performance liquid chromatography-tandem mass spectrometry].
    Author: Feng J, Jiang H, Wang J, Jing Z, Zhang F, Tan T, He F, Jiang L, Li H, Chang S, Li T.
    Journal: Se Pu; 2022 Sep; 40(9):843-853. PubMed ID: 36156631.
    Abstract:
    Chromatography combined with mass spectrometry is the most commonly used detection technology, and it offers the advantages of high sensitivity and high selectivity. The quick, easy, inexpensive, effective, rugged, and safe (QuEChERS) method is low-cost, effective, and time efficient. The application of the QuEChERS has now been extended to the analysis of contaminants in food samples. The aim of the study was to identify different concentration levels of multiple harmful drug residues in bean sprouts. In this study, QuEChERS coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for the simultaneous determination of 40 plant growth regulators, fungicides, insecticides, and antibiotics in bean sprouts. In the HPLC-MS/MS experiment, gibberellic acid, 4-fluorophenoxyacetic acid, chloramphenicol, N6-(δ2-isopentenyl)-adenine, 6-benzylaminopurine, 4-chlorophenoxyacetic acid, and 2,4-dichlorophenoxyacetic acid (2,4-D) were analyzed by MS/MS with negative electrospray ionization (ESI-). The other 33 target analytes (chlormequat, ronidazole, metronidazole, pymetrozine, dimetridazole, methomyl, carbendazim, enoxacin, levofloxacin, pefloxacin mesylate, norfloxacin, ciprofloxacin, enrofloxacin, thiabendazole, lomefloxacin, chlorpyrifos, sarafloxacin, imidacloprid, etc.) were analyzed by MS/MS with positive electrospray ionization (ESI+). Sensitive MS conditions were realized by optimizing the instrumental parameters such as the desolvent temperature, collision energy, spraying needle position, precursor ions, and product ions. Then, the optimal pretreatment method was determined by comparing the recovery rates of the 40 drugs obtained with different extraction solvents (methanol, acetonitrile, acetonitrile containing 0.1% ammonia, acetonitrile with 1% acetic acid), different extraction methods (ultrasonic extraction, shaking extraction), and purification with primary secondary amine (PSA) and C18. In this study, the bean sprouts samples were extracted twice by 10 mL acetonitrile with 1% acetic acid, and extracted under ultrasonic conditions. Then, the extracting solution was only cleaned with 100 mg C18. The chromatographic separation of the 40 compounds was accomplished on a Waters ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) with gradient elution. Methanol and 0.01% formic acid aqueous solution were used as the mobile phases. The 40 compounds were analyzed in the multiple reaction monitoring (MRM) mode. The matrix matching external standard method was used for quantitative determination. The results showed that the 40 compounds could be analyzed within 15 min. Under the optimized conditions, the calibration curves showed good linearities for the 40 compounds, and the coefficients of determination (r2) were greater than 0.99 in the range of 2-200 μg/L. The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.1-3 μg/kg and 0.3-9 μg/kg, respectively. Using negative bean sprouts as the substrates, the recovery tests were carried out at three spiked levels of 5, 10, and 50 μg/kg. The average recoveries of the 40 drugs were 78.5% to 115.3%, and the corresponding relative standard deviations (RSDs) were 1.3% to 9.7% (n=6). This method was successfully applied to the analysis of the 40 drug residues in 21 batches of local bean sprouts in Handan city. The results revealed the presence of extensive drug residues in the bean sprouts. The 26 batches were detected to varying degrees, among which 4-chlorophenoxyacetic acid, carbendazim, 6-benzyladenine, 2,4-D, enrofloxacin, and metronidazole were detected at high rates. The detection rates of 4-chlorophenoxyacetic acid, 6-benzyladenine, carbendazim, 2,4-D, gibberellic acid, and enrofloxacin were 28.6%, 19.0%, 9.5%, 9.5%, 4.8%, and 4.8%, respectively. The contents ranged from 37.5-352.4, 32.4-273.1, 28.8-38.7, 316.1-20.2, 19.9 and 13.6 μg/kg, respectively. Given its advantages of simplicity, rapidness, and high sensitivity, the developed method can be used for the rapid and accurate determination of trace levels of the 40 drug residues in large quantities of bean sprouts. 研究从豆芽质量安全监管的实际需求出发,建立了QuEChERS-高效液相色谱-串联质谱同时测定豆芽中植物生长调节剂、杀菌剂、杀虫剂和抗生素类等40种药物残留的方法。首先通过参数优化确定最佳质谱条件,然后比较不同提取溶剂(甲醇、乙腈、0.1%氨水乙腈、1%乙酸乙腈)、提取方法(超声、振荡)以及乙二胺-N-丙基硅烷化硅胶(PSA)、C18净化剂添加量时40种药物的回收率,确定最优前处理过程。样品用10 mL 1%乙酸乙腈提取两次,超声波辅助提取,100 mg C18为净化剂。选用Waters ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)进行分离,甲醇和0.01%甲酸水为流动相梯度洗脱,多反应监测(MRM)模式进行质谱监测,基质匹配外标法定量。结果表明,40种药物可在15 min内完成色谱分离,在2~200 μg/L的线性范围内均呈现出良好的线性关系,相关系数(r2)均大于0.99,检出限(LOD)和定量限(LOQ)分别为0.1~3 μg/kg和0.3~9 μg/kg。以阴性豆芽为基质,分别在5、10、50 μg/kg 3个水平下进行加标回收试验,40种药物的平均回收率为78.5%~115.3%,相对标准偏差(RSD)为1.3%~9.7%(n=6)。将该方法用于分析邯郸本地豆芽中40种药物的污染状况,结果显示4-氯苯氧乙酸、6-苄基腺嘌呤、多菌灵、2,4-二氯苯氧乙酸(2,4-D)、赤霉素和恩诺沙星检出率较高,分别为28.6%、19.0%、9.5%、9.5%、4.8%和4.8%,含量范围为37.5~352.4、32.4~273.1、28.8~38.7、16.1~20.2、19.9和13.6 μg/kg。研究建立的方法简单、快速,灵敏度高,适用于大批量豆芽中40种药物的快速准确测定。
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