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UPLC-MS法检测动物类药材中氯霉素类药物残留
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| 篇名： | UPLC-MS法检测动物类药材中氯霉素类药物残留 |
| TITLE： | |
| 摘要： | 目的：建立检测动物类药材中氯霉素类药物残留的方法。方法：采用超高效液相色谱-质谱法。色谱柱为SB-C18，流动相为乙腈-水（梯度洗脱），流速为0.2 mL/min，柱温为35 ℃，进样量为 20 μL；离子源为电喷雾离子源，干燥气温度为350 ℃，干燥气流量为5 L/min，鞘气温度为250 ℃，鞘气流量为11 L/min，毛细管电压为3 500 V，负离子扫描方式，多反应检测模式。结果：氯霉素、氟甲砜霉素和甲砜霉素检测质量浓度线性范围均为0.5～15 ng/mL（r分别为0.999 8、0.999 9、0.998 9）；定量限分别为0.03、0.03、0.15 μg/kg，检测限分别为0.01、0.01、0.05 μg/kg；精密度、稳定性、重复性试验的RSD＜3.0％；回收率分别为84.00％～112.80％（RSD＝10.15％，n＝9）、88.24％～109.80％（RSD＝7.11％，n＝9）、88.24％～99.02％（RSD＝3.91％，n＝9）。结论：该方法操作简便，精密度、稳定性、重复性好，可用于动物类药材中氯霉素类药物残留的检测。 |
| ABSTRACT： | OBJECTIVE：To establish the method for determination of chloramphenicol residue in animal medicinal herbs. METHODS： UPLC-MS method was adopted. The determination was performed on SB-C18 column with mobile phase consisted of acetonitrile-water （gradient elution） at the flow rate of 0.2 mL/min. The column temperature was 35 ℃， and sample size was 20 μL. The ion source was a jet stream ion focusing electrospray ion source. The temperature and flow of drying gas were 350 ℃ and 5 L/min， and those of sheath gas were 250 ℃， 11 L/min ，and capillary voltage was 3 500 V. Negative ion scanning mode was conducted with multiple reaction monitoring （MRM） mode. RESULTS： The linear ranges of thiamphenicol， florfenicol and chloramphenicol were 0.5-15 ng/ mL（r were 0.999 8，0.999 9，0.998 9，respectively）. The limits of quantitation were 0.03，0.03，0.15 μg/kg， and the limits of detection were 0.01，0.01，0.05 μg/kg. RSDs of precision， stability and reproducibility tests were all lower than 3.0％. The recoveries were 84.00％-112.80％（RSD＝10.15％，n＝9），88.24％-109.80％（RSD＝7.11％，n＝9），88.24％-99.02％（RSD＝3.91％，n＝9）。CONCLUSIONS： The method is simple， precise， stable and reproducible， and can be used for determination of chloramphenicol in animal medicinal herbs. |
| 期刊： | 2017年第28卷第30期 |
| 作者： | 张治军，周文杰，李志芸 |
| AUTHORS： | ZHANG Zhijun，ZHOU Wenjie，LI Zhiyun |
| 关键字： | 动物类药材；氯霉素类药物残留；超高效液相色谱-质谱法 |
| KEYWORDS： | Animal medicinal herbs； Chloramphenicol residue； UPLC-MS |
| 阅读数： | 317 次 |
| 本月下载数： | 16 次 |
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