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采用 DSPE/UPLC-MS/MS 法测定田间条件下青霉素 G 及其两种代谢物在柑橘中的消解和残留。

Dissipation and residue determination of penicillin G and its two metabolites in citrus under field conditions by DSPE/UPLC-MS/MS.

机构信息

Citrus Research Institute, Southwest University & Chinese Academy of Agricultural Sciences, Chongqing, China.

Laboratory of Citrus Quality and Safety Risk Assessment for Citrus Products, Ministry of Agriculture and Rural Affairs, Chongqing, China.

出版信息

Biomed Chromatogr. 2020 Dec;34(12):e4962. doi: 10.1002/bmc.4962. Epub 2020 Aug 26.

DOI:10.1002/bmc.4962
PMID:32783215
Abstract

A rapid determination method of residual penicillin G and its two metabolites in citrus was developed and validated by dispersive solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry (DSPE/UPLC-MS/MS). The samples were extracted with 80% acetonitrile and purified with octadecylsilane. High linearity was obtained with correlation coefficients (r ) >0.9981. The limits of quantification were 0.005-0.01 mg/kg. The recoveries of penicillin G and its metabolites spiked in blank citrus were within 76.7-107%, with relative standard deviations of 1.3-9.6%. The dissipation dynamics and distribution of penicillin G in citrus followed first-order kinetics, with half-life of 1.7-2.7 days. Penicillin G degraded easily in citrus and the metabolite was mainly penilloic acid, which can exist stably for long time. The terminal residues of penicillin G in pulp, whole citrus and peels were 0.015-0.701, 0.047-7.653 and 0.162-13.376 mg/kg, respectively. The hazard indexes for risk assessment of citrus were significantly <1, suggesting that the health risks to humans after consumption of citrus were insignificant and negligible. These results could provide necessary data for evaluating the safe and proper use of penicillin G in citrus.

摘要

建立了一种快速测定柑橘中残留青霉素 G 及其两种代谢物的方法,采用分散固相萃取和超高效液相色谱-串联质谱法(DSPE/UPLC-MS/MS)进行了验证。样品用 80%乙腈提取,用十八烷基硅烷纯化。青霉素 G 及其代谢物在空白柑橘中的添加回收率在 76.7-107%之间,相对标准偏差为 1.3-9.6%。青霉素 G 在柑橘中的消解动态和分布符合一级动力学,半衰期为 1.7-2.7 天。青霉素 G 在柑橘中容易降解,代谢物主要为苯氧乙酸,可长期稳定存在。青霉素 G 在果肉、整个柑橘和果皮中的最终残留量分别为 0.015-0.701、0.047-7.653 和 0.162-13.376 mg/kg。风险评估的危害指数显著<1,表明人类食用柑橘后青霉素 G 的健康风险不显著,可忽略不计。这些结果可为评估青霉素 G 在柑橘中的安全合理使用提供必要的数据。

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