禽畜肉中7种抗生素残留检测
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摘要
使用超高效液相色谱(UPLC)技术建立禽畜肉中7种抗生素残留的分析方法。使用乙腈水体系提取样品,乙腈饱和正己烷除脂,低温高速离心,UPLC检测,外标法定量。7种抗生素在24～100 ng/g线性关系良好,相关系数均高于0. 999;土霉素、四环素、多西环素和氯霉素的检测限为5 ng/g,定量限为16. 67 ng/g;阿莫西林、金霉素和氟苯尼考的检测限为7 ng/g,定量限为23. 33 ng/g; 7种抗生素的加样回收率在80. 0%～98. 0%之间,且RSD均低于6. 0%。
Ultra-high performance liquid chromatography(UPLC) technology was used to establish a residue analysis method for seven antibiotics in poultry meat. The sample was extracted with acetonitrile/H2 O system and defatted with n-hexane saturated by acetonitrile. After low-temperature high-speed centrifugation,the sample was analyzed by UPLC. The qualification was based on external standard method. The linearity of the seven antibiotics ranged from 24 to 100 ng/g,and the correlation coefficients were higher than 0. 999. The limits of detection(LODs) of oxytetracycline,tetracycline,doxycycline and chloramphenicol were all 5 ng/g,and the limits of quantification(LOQs) were16. 67 ng/g; LODs of amoxicillin,chlortetracycline and florfenicol were 7 ng/g and LOQs were23. 33 ng/g; the recoveries of 7 antibiotics were between 80. 0%-98. 0%, with RSDs bower than 6. 0%.
Ultra-high performance liquid chromatography(UPLC) technology was used to establish a residue analysis method for seven antibiotics in poultry meat. The sample was extracted with acetonitrile/H2 O system and defatted with n-hexane saturated by acetonitrile. After low-temperature high-speed centrifugation,the sample was analyzed by UPLC. The qualification was based on external standard method. The linearity of the seven antibiotics ranged from 24 to 100 ng/g,and the correlation coefficients were higher than 0. 999. The limits of detection(LODs) of oxytetracycline,tetracycline,doxycycline and chloramphenicol were all 5 ng/g,and the limits of quantification(LOQs) were16. 67 ng/g; LODs of amoxicillin,chlortetracycline and florfenicol were 7 ng/g and LOQs were23. 33 ng/g; the recoveries of 7 antibiotics were between 80. 0%-98. 0%, with RSDs bower than 6. 0%.
引文
[1] Liu L N. Chin. Abstr. Animal Husbandry and Veterinary Medicine,2018,34(1):24刘丽娜.中国畜牧兽医文摘,2018,34(1):24.
[2] Wang A B,Sun S,Yang M,et al. Animal Husbandry and Veterinary Medicine,2017,33(5):230.王安波,孙思,杨梅,等.中国畜牧兽医文摘,2017,33(5):230
[3] GB/T 21317—2007 Determination of tetracyclines residues in food of animal origin-LC-MS/MS method and HPLC method GB/T 21317—2007动物源性食品中四环素类兽药残留量检测方法液相色谱-质谱/质谱法
[4] GB/T 20756—2006 Method for the determination of chloramphenicol thiamphenicol,and florfenicol residues in edible animal muscles liver and aquatic products-LC-MS-MS method GB/T 20756—2006可食动物肌肉、肝脏和水产品中氯霉素、甲砜霉素和氟苯尼考残留量的测定液色谱-串联质谱法
[5] GB/T 20755—2006 Method for the determination of nine penicillins residues in livestork and poultry muscles-LC-MSMS method GB/T 20755—2006畜禽肉中九种青霉素类药物残留量的测定液相色谱-串联质谱法
[6] Gao F D,Zhao Y,Shao B,et al. Chinese J. Chrom.,2012,30(6):560高馥蝶,赵妍,邵兵,等.色谱,2012,30(6):560
[7] Yu L,Sun W,Lv Y N,et al. Chinese J. Chrom.,2015,33(6):597余璐,宋伟,吕亚宁,等.色谱,2015,33(6):597
[8] Zhang L T,Huang S Y,Yang X,et al. Chinese J. Anal. Lab.,2015,34(12):1403张林田,黄少玉,杨晞,等.分析试验室,2015,34(12):1403
[9] Xu W,Zhang X Y,Wu B,et al. Chinese J. Chrom.,2012,30(10):1089许蔚,张晓燕,吴斌,等.色谱,2012,30(10):1089
[10] Wang Y D,Liu J,Wang G N,et al. Animal Husbandry and Veterinary Medicine,2016,43(6):1579王旭丹,刘静,王庚南,等.中国畜牧兽医文摘,2016,43(6):1579
[11] Liang J N,Cao P,Zhang X Q,et al. Chin. J. Anal. Lab.,2017,36(12):1411梁君妮,曹鹏,张禧庆,等.分析试验室,2017,36(12):1411
[12] Pan J,Yan F,Gu X,et al. Chin. J. Vet. Drug,2015,49(4):56潘娟,严凤,顾欣.中国兽药杂志,2015,49(4):56
[13] Duan L Q,Wang J,Cao R D,et al. Chin. J. Anal. Lab.,2018,37(7):843端礼钦,王静,曹润冬,等.分析试验室,2018,37(7):843
[14] Wang S,Zhang J,Shao B,et al. J. Instr. Anal.,2013,32(2):179王硕,张晶,邵兵,等.分析测试学报,2013,32(2):179
[15] Yang Q H,Ai X H,Li R,et al. Chin. J. Anal. Lab.,2015,34(5):533杨秋红,艾晓辉,李荣,等.分析试验室,2015,34(5):533
[16] Announcement of the Ministry of Agriculture of the People's Republic of China. No. 235 Maximum Residue Limits for Veterinary Drugs in Animal Foods.,2002中华人民共和国农业部公告.第235号动物性食品中兽药最高残留限量,2002
[2] Wang A B,Sun S,Yang M,et al. Animal Husbandry and Veterinary Medicine,2017,33(5):230.王安波,孙思,杨梅,等.中国畜牧兽医文摘,2017,33(5):230
[3] GB/T 21317—2007 Determination of tetracyclines residues in food of animal origin-LC-MS/MS method and HPLC method GB/T 21317—2007动物源性食品中四环素类兽药残留量检测方法液相色谱-质谱/质谱法
[4] GB/T 20756—2006 Method for the determination of chloramphenicol thiamphenicol,and florfenicol residues in edible animal muscles liver and aquatic products-LC-MS-MS method GB/T 20756—2006可食动物肌肉、肝脏和水产品中氯霉素、甲砜霉素和氟苯尼考残留量的测定液色谱-串联质谱法
[5] GB/T 20755—2006 Method for the determination of nine penicillins residues in livestork and poultry muscles-LC-MSMS method GB/T 20755—2006畜禽肉中九种青霉素类药物残留量的测定液相色谱-串联质谱法
[6] Gao F D,Zhao Y,Shao B,et al. Chinese J. Chrom.,2012,30(6):560高馥蝶,赵妍,邵兵,等.色谱,2012,30(6):560
[7] Yu L,Sun W,Lv Y N,et al. Chinese J. Chrom.,2015,33(6):597余璐,宋伟,吕亚宁,等.色谱,2015,33(6):597
[8] Zhang L T,Huang S Y,Yang X,et al. Chinese J. Anal. Lab.,2015,34(12):1403张林田,黄少玉,杨晞,等.分析试验室,2015,34(12):1403
[9] Xu W,Zhang X Y,Wu B,et al. Chinese J. Chrom.,2012,30(10):1089许蔚,张晓燕,吴斌,等.色谱,2012,30(10):1089
[10] Wang Y D,Liu J,Wang G N,et al. Animal Husbandry and Veterinary Medicine,2016,43(6):1579王旭丹,刘静,王庚南,等.中国畜牧兽医文摘,2016,43(6):1579
[11] Liang J N,Cao P,Zhang X Q,et al. Chin. J. Anal. Lab.,2017,36(12):1411梁君妮,曹鹏,张禧庆,等.分析试验室,2017,36(12):1411
[12] Pan J,Yan F,Gu X,et al. Chin. J. Vet. Drug,2015,49(4):56潘娟,严凤,顾欣.中国兽药杂志,2015,49(4):56
[13] Duan L Q,Wang J,Cao R D,et al. Chin. J. Anal. Lab.,2018,37(7):843端礼钦,王静,曹润冬,等.分析试验室,2018,37(7):843
[14] Wang S,Zhang J,Shao B,et al. J. Instr. Anal.,2013,32(2):179王硕,张晶,邵兵,等.分析测试学报,2013,32(2):179
[15] Yang Q H,Ai X H,Li R,et al. Chin. J. Anal. Lab.,2015,34(5):533杨秋红,艾晓辉,李荣,等.分析试验室,2015,34(5):533
[16] Announcement of the Ministry of Agriculture of the People's Republic of China. No. 235 Maximum Residue Limits for Veterinary Drugs in Animal Foods.,2002中华人民共和国农业部公告.第235号动物性食品中兽药最高残留限量,2002