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建立了中华鳖(Trionyx sinensis)组织(血浆、肌肉、裙边、肝脏和肾脏)中氯硝柳胺、氯霉素、甲砜霉素、氟苯尼考和氟苯尼考胺同时测定的高效液相色谱-加热电喷雾电离源串联质谱法(HPLC-HESI/MS/MS)。样品经改进的QuEChERS方法提取净化,以氨化乙腈为提取剂,十八烷基硅烷键合硅胶(C18)粉为净化剂,甲醇-水为流动相,流速为0.3mL/min,以Waters Symmetry C18(2.1mm×100mm,3.5μm)为色谱分离柱,采用正负离子分段扫描和多反应监测模式(MRM)检测。氯霉素、甲砜霉素、氟苯尼考和氟苯尼考胺采用内标标准曲线法定量,氯硝柳胺采用基质匹配标准曲线外标法定量。结果表明,在0.3~100μg/L范围内,5种待测物均呈良好的线性关系,相关系数(r2)均不小于0.9987。在1~20μg/kg加标水平下,中华鳖空白血浆、肌肉、裙边、肝脏和肾脏的加标回收率为77.9%~105.3%(n=6),相对标准偏差为2.7%~10.5%(n=6),方法的检出限分别为0.5、0.1、0.5、0.5、0.5μg/kg,定量下限分别为1.0、0.3、1.0、1.0、1.0μg/kg。该方法操作简便、准确、灵敏度高,适用于中华鳖组织中氯硝柳胺、氯霉素、甲砜霉素、氟苯尼考和氟苯尼考胺残留量的同时测定。
The simultaneous determination of niclosamide, chloramphenicol, thiamphenicol, florfenicol and florfenicol in Trionyx sinensis tissues (plasma, muscle, skirt, liver and kidney) was established Liquid chromatography-electrospray ionization-electrospray ionization tandem mass spectrometry (HPLC-HESI / MS / MS). The samples were purified by QuEChERS method. Ammonia acetonitrile was used as the extractant, and C18 powder was used as decontaminant. The mobile phase consisted of methanol and water with a flow rate of 0.3 mL / C18 (2.1mm × 100mm, 3.5μm) for the chromatographic separation column, using positive and negative ion segmentation scanning and multiple reaction monitoring mode (MRM) detection. Chloramphenicol, thiamphenicol, florfenicol and florfenicol amine were quantified by internal standard curve method, and niclosamide was quantified by matrix matching standard curve external standard method. The results showed that in the range of 0.3 ~ 100μg / L, the five kinds of analytes showed a good linear relationship, the correlation coefficient (r2) was not less than 0.9987. The spiked recoveries of blank plasma, muscle, skirt, liver and kidney of Chinese turtle were 77.9% -105.3% (n = 6) with relative standard deviations of 2.7% -10.5% at the spiked level of 1 ~ 20μg / (n = 6). The detection limits were 0.5, 0.1, 0.5, 0.5 and 0.5 μg / kg respectively, and the lower limits of quantitation were 1.0, 0.3, 1.0, 1.0 and 1.0 μg / kg, respectively. The method is simple, accurate and sensitive, and is suitable for the simultaneous determination of niclosamide, chloramphenicol, thiamphenicol, florfenicol and florfenicol in Chinese soft-shelled turtle.