UPLC-MS法检测动物类药材中氯霉素类药物残留  

Determination of Chloramphenicol Residue in Animal Medicinal Herbs by UPLC-MS

作　　者：张治军[1] 周文杰[1] 李志芸 ZHANG Zhijun ZHOU Wenjie LI Zhiyun(Guangxi Guilin Institute for Food and Drug Control, Guangxi Guilin 541001, China College of Pharmacy,Guilin Medical University, Guangxi Guilin 541004, China)

机构地区：[1]广西壮族自治区桂林食品药品检验所,广西桂林541001 [2]桂林医学院药学院,广西桂林541004

出　　处：《中国药房》2017年第30期4271-4274,共4页China Pharmacy

基　　金：广西壮族自治区食品药品监督管理局科研项目(No.桂食药监科评函[2015]20号)

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-C_(18),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20μL;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、0.15μg/kg,检测限分别为0.01、0.01、0.05μg/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。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-C_（18） 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 20μL. The ion source was a jet stream ion focusing electrospray ion source. The temperature and flow of drying gas were 350 ℃ and5 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 than3.0%. 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.

关 键 词：动物类药材 氯霉素类药物残留 超高效液相色谱-质谱法 

分 类 号：R927[医药卫生—药学]