亚临界水萃取-HPLC法测定动物源食品中土霉素、四环素和氯霉素残留量  

Detection of Residual Oxytetracycline, Tetracycline and Chloramphenicol in Animal Foodstuff by Subcritical Water Extraction-HPLC

作　　者：徐万帮 胡音 洪建文 杨立伟 

机构地区：[1]广东省食品药品检验所,广州510180

出　　处：《中国药房》2013年第25期2356-2359,共4页China Pharmacy

基　　金：广东省食品药品监督管理局系统课题资助项目(No.ZA20101518)

摘　　要：目的:建立一种快速、简单、灵敏的动物源食品中土霉素、四环素和氯霉素残留量的测定方法。方法:采用亚临界水(饱和硼砂水溶液)萃取-高效液相色谱法。优化萃取条件;色谱柱为ZORBAXSB-C18,流动相为0.01mol/L磷酸氢二钠+0.001mol/L乙二胺四乙酸二钠(pH2.5)-乙腈(75∶25,V/V),流速为1.0ml/min,检测波长为270nm,柱温为30℃。检测6种动物源样品(鸡肉、猪肉、牛肉、鱼、猪内脏、鸡内脏)共56份中的土霉素、四环素和氯霉素残留量。结果:萃取最优条件是取5ml用盐酸调节pH至2.0的饱和硼砂水溶液为萃取剂,在100℃萃取5min;此条件下土霉素、四环素和氯霉素的萃取回收率分别为104.8%、99.7%、92.1%(n=3)。方法学考察中土霉素、四环素、氯霉素的检测限分别为3.6、5.0、2.0ng/ml,回收率分别为99.8%、100.5%、97.6%(RSD分别为0.3%、0.3%、0.5%)。共检出8份样品呈阳性。结论:建立的方法萃取时间短,准确、可靠、灵敏度高,分析效率较高。OBJECTIVE： To establish a rapid, simple and sensitive method for the determination of residual oxytetracycline （OTC）, tetracycline（TC） and chloramphenicol （CPA） in animal foodstuff. METHODS： Subcritical water （saturated borax solution） extraction-HPLC method was adopted. The extracting condition was optimized; ZORBAX SB-C18 column was adopted, with 0.01 mol/L sodium dihydrogen phosphate＋0.001 mol/L EDTA （pH 2.5）-acetonitrile （75 ∶ 25, V/V） as mobile phase and flow rate of 1.0 ml/min, detection wavelength of 270 nm, column temperature of 30 ℃. The residual contents of OTC, TC and CPA in 56 samples from 6 kinds of animal samples （chicken, pork, beef, fish, haslet and chicken offal） were all determined. RESULTS： Optimal extraction condition was as follows： pH of 5 ml saturated borax solution adjusted to 2.0 using hydrochloric acid as extracting agent, extracting for 5 min at 100 ℃; the recovery rates of TC, OTC and CAP were 104.8%, 99.7%, 92.1% respectively （n=3）. In methodology study, the limits of detection of TC, OTC and CAP were 3.6 ng/ml, 5.0 ng/ml and 2.0 ng/ml, and recovery rates were 99.8% （RSD=0.3%）, 100.5% （RSD=0.3%） and 97.6% （RSD=0.5%）. 8 samples were positive in the study. CONCLUSIONS： The method is accurate, reliable and sensitive with short extraction time and high analysis efficiency.

关 键 词：亚临界水萃取 高效液相色谱法 土霉素 四环素 氯霉素 动物源食品 残留量 

分 类 号：R978.13[医药卫生—药品] R978.14[医药卫生—药学]