液—质联用法检测乳品中六种聚醚类抗生素的残留
|
摘要
聚醚类抗生素又称离子载体抗生素,是目前广泛使用的高效、广谱抗球虫药,也可作为畜禽的促生长剂。过量地使用这种抗生素会导致动物产品中残留,甚至会造成畜禽动物的中毒或死亡。
本研究以外标法为定量手段,以全脂牛奶、低脂牛奶、鲜牛奶、全脂奶粉、婴儿钙化奶粉、脱脂奶粉为材料,建立了一种专属、灵敏的超高效液相色谱-串接质谱法检测六种聚醚类抗生素残留的分析方法。
结果表明:
1.二氯甲烷、甲醇和乙酸乙酯作为提取剂时,样品的平均回收率在10.52%～70.13%,而乙腈作为提取剂时,样品的平均回收率均可达到70%以上,确定提取溶剂为乙腈。
2.固相萃取法和凝胶渗透色谱法作为净化方法时,样品的平均回收率在15.21%～65.40%,而液液萃取法作为净化方法时,样品的平均回收率均可达到71.20%以上,故选取液液萃取法作为净化方法。
3.色谱条件为:色谱柱温度40℃;流速0.25 mL /min;流动相甲醇+0.1%甲酸-5 mmol/L的乙酸铵(90:10,v:v);进样量:5.0μL。质谱条件:毛细管电压2.8 KV;离子源温度110℃;去溶剂气温度380℃;去溶剂气(氮气)流量600 L/hr。
4.在此条件下,六种抗生素在0.5μg/Kg～100μg/Kg浓度范围内呈线性,相关系数r>0.99。在空白样品中,添加拉沙洛素、莫能菌素、尼日利亚菌素、盐霉素、甲基盐霉素和马杜拉霉素的回收率分别在75.62%～112.55%、78.25%～112.13%、74.89%～108.10%、78.11%～108.94%、74.60%～114.20%、78.70%～115.64%之间,精密度(RSD)分别为4.97%～12.88%、3.91%～13.76%、5.34%～13.68%、4.40%～13.94%、4.19%～13.42%、3.94%～12.59%之间,最低检测限分别为0.2μg/Kg、0.1μg/Kg、0.1μg/Kg、0.2μg/Kg、0.1μg/Kg、0.3μg/Kg。
本实验建立方法可应用于牛奶和奶粉中六种聚醚类抗生素残留的检测。
Polyether antibiotics, also known as ionophore antibiotic, was widely used as high- efficiency, broad-spectrum anti-Coccidiostats, can also be used as animal growth-promoting agent. To use this antibiotics excessiveLy will lead to residues in animal food, or even cause animal poisoning or death.
In this study, Selected full fat milk, low fat milk, fresh milk, full fat powdered milk, calcification of powdered milk for infant, skimmed fat milk as samples, a sensitive and selective method was developed for determination of six Polyether antibiotics residues in milk and powdered milk. Using external standard method.
The results show:
First: Dichloromethane, methanol and ethyl acetate as extractions, the average recovery rate of samples between 10.52% and 70.13%, but acetonitrile as the extraction, the average recovery rate of samples was over 70%, so the extraction was acetonitrile. Second: Solid-phase extraction method and gel permeation chromatography as a clean-up method, the average recovery rate of samples between 15.21% and 65.40%, but liquid-liquid extraction as a clean-up method, the average recovery rate of samples was over 71.20%, so liquid-liquid extraction was the clean-up method.
Third: Chromatographic conditions: Methanol +Formic acid of 0.1%-Ammonium acetate of 5 mmol/L (90:10,v:v) as its mobile, the flow rate was 0.25 mL/min, column temperature was at 40℃. MS conditions: the capillary cone was 2.8 KV; ion source temperature was 110℃; desolvation temperature was 380℃; desolvation gas flow was 600 L/hr.
Fourth: The operating ranges of the chromatographic analysis were determined. Calibration graphs were good linearity over the concentration ranges tested (0.5μg/Kg～100μg/Kg, R>0.99). The average recoveries from spiked milk and powdered milk at the three concentrations of 0.5, 10.0, 20.0μg/Kg ranged from 75.62%～112.55%、78.25%～112.13%、74.89%～108.10%、78.11%～108.94%、74.60%～114.20%、78.70%～115.64% respectively; with relative standard deviation ranged from 4.97%～12.88%、3.91%～13.76%、5.34%～13.68%、4.40%～13.94%、4.19%～13.42%、3.94%～12.59% respectively; and the limits of detection were 0.2μg/Kg、0.1μg/Kg、0.1μg/Kg、0.2μg/Kg、0.1μg/Kg、0.3μg/Kg respectiveLy in milk and powdered milk.
Our experiment used liquid chromatography with mass pectrometry was confirmed, it was applied to detect six Polyether antibiotics residual in milk and powdered milk.
本研究以外标法为定量手段,以全脂牛奶、低脂牛奶、鲜牛奶、全脂奶粉、婴儿钙化奶粉、脱脂奶粉为材料,建立了一种专属、灵敏的超高效液相色谱-串接质谱法检测六种聚醚类抗生素残留的分析方法。
结果表明:
1.二氯甲烷、甲醇和乙酸乙酯作为提取剂时,样品的平均回收率在10.52%～70.13%,而乙腈作为提取剂时,样品的平均回收率均可达到70%以上,确定提取溶剂为乙腈。
2.固相萃取法和凝胶渗透色谱法作为净化方法时,样品的平均回收率在15.21%～65.40%,而液液萃取法作为净化方法时,样品的平均回收率均可达到71.20%以上,故选取液液萃取法作为净化方法。
3.色谱条件为:色谱柱温度40℃;流速0.25 mL /min;流动相甲醇+0.1%甲酸-5 mmol/L的乙酸铵(90:10,v:v);进样量:5.0μL。质谱条件:毛细管电压2.8 KV;离子源温度110℃;去溶剂气温度380℃;去溶剂气(氮气)流量600 L/hr。
4.在此条件下,六种抗生素在0.5μg/Kg～100μg/Kg浓度范围内呈线性,相关系数r>0.99。在空白样品中,添加拉沙洛素、莫能菌素、尼日利亚菌素、盐霉素、甲基盐霉素和马杜拉霉素的回收率分别在75.62%～112.55%、78.25%～112.13%、74.89%～108.10%、78.11%～108.94%、74.60%～114.20%、78.70%～115.64%之间,精密度(RSD)分别为4.97%～12.88%、3.91%～13.76%、5.34%～13.68%、4.40%～13.94%、4.19%～13.42%、3.94%～12.59%之间,最低检测限分别为0.2μg/Kg、0.1μg/Kg、0.1μg/Kg、0.2μg/Kg、0.1μg/Kg、0.3μg/Kg。
本实验建立方法可应用于牛奶和奶粉中六种聚醚类抗生素残留的检测。
Polyether antibiotics, also known as ionophore antibiotic, was widely used as high- efficiency, broad-spectrum anti-Coccidiostats, can also be used as animal growth-promoting agent. To use this antibiotics excessiveLy will lead to residues in animal food, or even cause animal poisoning or death.
In this study, Selected full fat milk, low fat milk, fresh milk, full fat powdered milk, calcification of powdered milk for infant, skimmed fat milk as samples, a sensitive and selective method was developed for determination of six Polyether antibiotics residues in milk and powdered milk. Using external standard method.
The results show:
First: Dichloromethane, methanol and ethyl acetate as extractions, the average recovery rate of samples between 10.52% and 70.13%, but acetonitrile as the extraction, the average recovery rate of samples was over 70%, so the extraction was acetonitrile. Second: Solid-phase extraction method and gel permeation chromatography as a clean-up method, the average recovery rate of samples between 15.21% and 65.40%, but liquid-liquid extraction as a clean-up method, the average recovery rate of samples was over 71.20%, so liquid-liquid extraction was the clean-up method.
Third: Chromatographic conditions: Methanol +Formic acid of 0.1%-Ammonium acetate of 5 mmol/L (90:10,v:v) as its mobile, the flow rate was 0.25 mL/min, column temperature was at 40℃. MS conditions: the capillary cone was 2.8 KV; ion source temperature was 110℃; desolvation temperature was 380℃; desolvation gas flow was 600 L/hr.
Fourth: The operating ranges of the chromatographic analysis were determined. Calibration graphs were good linearity over the concentration ranges tested (0.5μg/Kg～100μg/Kg, R>0.99). The average recoveries from spiked milk and powdered milk at the three concentrations of 0.5, 10.0, 20.0μg/Kg ranged from 75.62%～112.55%、78.25%～112.13%、74.89%～108.10%、78.11%～108.94%、74.60%～114.20%、78.70%～115.64% respectively; with relative standard deviation ranged from 4.97%～12.88%、3.91%～13.76%、5.34%～13.68%、4.40%～13.94%、4.19%～13.42%、3.94%～12.59% respectively; and the limits of detection were 0.2μg/Kg、0.1μg/Kg、0.1μg/Kg、0.2μg/Kg、0.1μg/Kg、0.3μg/Kg respectiveLy in milk and powdered milk.
Our experiment used liquid chromatography with mass pectrometry was confirmed, it was applied to detect six Polyether antibiotics residual in milk and powdered milk.
引文
[1]贺家亮,李开雄,于见亮,等.动物性食品兽药残留现状及对策[J].中国动物检疫, 2006, 23(7): 22-24
[2]佟恒敏,李艳华,韩建春.我国动物性食品中兽药残留的现状及为危害[J].黑龙江畜牧兽医,2003, 11, 61-62
[3]吕秀娟.降低畜禽药物残留的基本原则[J].兽药导刊, 2008, 7: 39-40
[4]胡登兵,丁新建,张焕容.兽药残留危害及国内外一般控制措施[J].四川畜牧兽医, 2008,河南畜牧兽医, 2003, 9(24): 21
[5]马艳梅.动物性食品兽药残留及控制措施[J] .江西畜牧兽医杂志, 2005, 1: 37-38
[6]贾久满,贾长江,石洪凌.动物性食品中抗生素残留对青少年儿童肥胖的影响[J].中华实用中西医杂志, 2004, 17(4): 1397-1398
[7]丁全福主编.药理学[M].北京:人民出版, 2001, 249-250
[8]李红,张莹蕾,李永军,马伟华.高效液相色谱法测定牛奶中氯霉素残留的研究综述[J].河南畜牧兽医, 2007, 28(2): 11
[9]吴祥集.动物性食品中兽药残留对人体健康的危害及其控制[J].贵州畜牧兽医, 2006, 30(3) : 25-27
[10]李娜.鸡组织中三种聚醚类抗生素残留的微生物法检测研究[D].安徽农业大学, 2007
[11]刘忠琛,张建波,管瑛,等.畜产品药物残留的危害及控制策略[J].广州饲料, 2004, 2(13): 9-11
[12]中华人民共和国农业部,关于发布《动物性食品中兽药最高残留限量》的通知, 1999-9-13, http://www.agri.gov.cn/xumugb/99-2-2.htm
[13]沈建忠,何继红.浅谈兽药残留分析技术研究进展[J].中国禽业导刊, 2004, 21: 15-16
[14]胡登兵,丁新建,张焕容.兽药残留危害及国内外一般控制措施[J].四川畜牧兽医, 2008,河南畜牧兽医, 2003, 9(24): 21
[15]欧盟抗生素残留仍然不可忽视[J] .中国动物保健, 2006, 6: 57
[16]张许科,刘兴金.国内外兽药发展趋势及对策[J] .中国家禽2004, 24(7): 1-4
[17] Kim S, Carlson K. Quantification of human and veterinary antibiotics in water and sediment using SPE/LC/MS/MS[J]. Anal. Bioanal. Chem., 2007, 387: 1301-1305
[18] Dimenna G P, Creegan J A, Turnbull L B. et al. Determination of Sodium salinomycin in chicken skin/fat by High-performance liquid chromatography utilizing column switching and UV detection[J]. J. Agric. Food Chem., 1986, 34(5): 805-810
[19] Elissalde M H, Beier R C, Rowe L D, et al. Development of a Monoclonal-based enzyme-linked immunosorbent assay for the coccidiostat salinomycin[J]. J. Agric. Food Chem., 1993, 41(11): 2167-2171
[20] Blanchflower W J, Kenndy D G. Determination of monensin, salinomycin and narasin in muscle, liver and eggs from domestic fowl using liquid chromatography-electrospray mass spectrometry[J]. J. Chromatogr. B, 1996, 675: 225-230
[21]商军,吴霞云,顾欣.莫能菌素微生物检定法的改进[J].中国兽药杂志, 1999, 33(1): 7-9
[22] Berger J, Rachlin A I, Scott W E, et al. The isolation of three crystalline antibiotics from Streptomyces[J]. J. Am. Chem. Soc., 1951, 73: 5295～5298
[23]Mallams A. K. Antibiotics(Polyethers)[J]. In Encyclopedia of Chemical Technology, Wiley: New York, 1978, 3: 47-63
[24]阎晓菊,顾觉奋.聚(多)醚类抗生素(综述) [J].现代应用药学, 1987, 4(4): 43-46
[25]杨桂香,曾振灵,陈杖榴.聚醚类抗生素对肉鸡的毒性作用及其合理应用[J].养禽与禽病防治, 2001, 2: 13-14
[26]吕爱军,穆阿丽,宋小敬,等.聚醚类抗生素的作用机理及应用研究进展[J].吉林畜牧兽医. 2004, 5: 22-24
[27]倪月菊.日本“肯定列表制度”的实施及其对我国食品和农产品的影响[J].国际贸易, 2006, 7: 22-25
[28]陈明,耿志明,王冉,等.饲料中聚醚类抗生素的柱后衍生同时测定方法研究[J].中国饲料,2005, 20: 27-29
[29]Martin D R, Rowley L, Shearer G, et al. Effect of cooking on Veterinary drug residues in food. 6. Lasalocid[J]. J. Agric. Food Chem., 1997, 45(3): 927
[30]李娜,祁克宗,朱良强等.聚醚类抗生素残留检测方法的研究进展[J].家禽科学,2007,5:38-40
[31]霍晓荣,刘铁铮,王冉,等.盐霉素和莫能菌素残留分析方法的研究进展[J].中国畜牧兽医, 2005, 32(7): 23-24
[32]肖琳,黄为一.尼日利亚菌素高产菌株的选育[J].微生物学通报, 2002, 29(4): 59
[33]罗洁,谢天尧,刘秋英,等.聚醚类抗生素盐霉素的毛细管电泳-电导分离检测研究[C] .第三届全国微全分析系统学术会议论文集, 2005, 10: 246-247
[34] Miyazaki Y, Shibuya M, Sugawara H, et al. Salinomycin, a new Polyether antibiotic[J]. J. Antibiot, 1974, 11: 814-821
[35]李启琳,李燕鹏,王士长.鸡肉中残留盐霉素的高效液相色谱检测法[J].农产品加工, 2007, 10: 67-68
[36]沈建忠,钱传范,杨汉春,等.马杜霉素在鸡组织中残留检测方法的研究[J].畜牧兽医学报, 1999, 30(2) :172-179
[37]周伟伟,卜仕金.聚醚类离子载体抗生素的研究进展[J].兽药与饲料添加剂, 2006, 11(3) :13-15
[38]杨桂香,陈杖榴.聚醚类抗生素毒性研究进展[J] .动物医学进展, 2000, 2( 4) : 2-5
[39] Badiola J J, Luco D F, Perz M A, et al. Mauduramycin and tiamulin compatibility in broiler chickens[J]. Avian Patho., 1994, 23: 3-17
[40]马学海,施玉樑.离子载运体的大家族-多醚类抗生素[J].生物学通报,1996,31(6):1-3
[41]朱模忠.兽药手册[M]. 1版.北京:化工出版社, 2002: 194-197
[42]刘继业,苏晓欧.饲料安全工作手册[M].北京:中国农业出版社, 2001: 17-40
[43]张丹红,王恩,周元林.莫能菌素中毒致横纹肌溶解症三例[J].中华神经科杂志,2006, 39(2) : 88
[44]刘燕,高萍.莫能菌素中毒致多器官功能障碍4例的护理体会[J]. 2005, 31 (6): 430-431
[45]潘蕴慈,董金芝,边景荣,等.盐霉素对肉鸡残留量的测定[J].科学试验与研究, 1992, 9: 8-9
[46]Cabadaj R, Nagy J, Popelka P, et al. The determination of Salinomycin residues in the tissues of broiler chickens by using microbiological diffusion methods[J]. Slove. Vet. Res., 2002, 39 (2): 137-143
[47]Kozarova I, Mate D, Cabadaj R et al. An evaluation of the microbiological diffusion methods as a tool for screening monensin residues in the tissues of broiler chickens[J]. Folia Vet., 2002,46(1): 27-33
[48]李俊锁,邱月明,王超.兽药残留分析[M].上海:上海科技出版社, 2002:538-550
[49]国家药典委员会.中华人民共和国药典(二部,附录Ⅺ)[M].北京化学工业出版社,2005: 22-24
[50]Golab T, Barton S J, Scroggs R E. Colorimetric method for monensin[J]. J. Assoc. Off Anal. Chem., 1973, 56(1): 171-173
[51]Owles P J. Identification of monensin, narasin, salinomycin and lasalocid in pre-mixes and feeds by thin-layer chromatography[J]. Anal., 1984, 109(10):1331-1333
[52]Landgraf W W, Ross F P. Thin-layer chromatographic determination of monensin in feeds: screening method[J]. J. AOAC Int, 1998, 81(4): 844-847
[53]陈运勤,李跃龙,伍绍登,等.用薄层扫描法测定马杜霉素残留[J].中国动物保健, 2003, 7: 21-23
[54]Martinez E E, Shimoda W. Identification and semiquantitation of monensin sodium in animal feeds by thin layer bioautography[J]. J. Assoc. Off Anal. Chem., 1983, 66(6): 1506-1509
[55]VanderKop P A, MacNeil J D. Separation and detection of monensin, salinomycin and lasalocid in animal feeds by thin layer bioautography[J]. J. Chromatogr. A, 1990, 508(2): 386-390
[56]农业部.动物源食品中莫能菌素和盐霉素残留检测方法-高效液相色谱法[J].中国兽药杂志, 2002, 36(8): 9-10
[57]张素霞,沈建忠,吕亚滨,等.莫能菌素和盐霉素在鸡组织中的残留分析方法研究[J].畜牧兽医学报, 2000, 31(6): 530-535
[58]陈笑梅,施旭霞.柱后衍生高效液相色谱法测定鸡肉中莫能菌素残留量[J].色谱, 1999, 17(1): 77-79
[59]项新华,涂晓明,贾明宏,等.高效液相色谱法检测动物组织中马杜霉素残留[J].中国公共卫生, 2002, 18(1): 101-102
[60]Blanchflower W J, Rice D A, HamiLton J T. Simultaneous high-performance liquid chromatographic determination of monensin, narasin and salinomycin in feeds using post-column derivatisation[J]. Anal., 1985, 110(11): 1283-1287
[61]Dusi G, Gamba V. Liquid chromatography with ultraviolet detection of lasalocid , monensin, salinomycin and narasin in poultry using pre-column derivatization[J]. J. Chromatogr. A, 1999, 835: 243-246
[62]Hormazábal V, Yndestad M. Ostensvik O.Determination of amprolium, ethopabate, lasalocid, monensin, narasin and salinomycin in chicken tissues, plasma, and egg using liquid chromatography-mass spectrometry[J]. Liqu. Chromatogr. Related Tech., 2002, 23(10): 585-1598
[63]Heller D N, Nochetto C B. Development of multiclass methods for drug residues in eggs: silica SPE cleanup and LC-MS/MS analysis of lonophore and macrolode residues[J]. J. Agric. Food Chem., 2004, 52(23): 6848-6856
[64]Mortier L, Daeseleire E, Peteghem C V. Determination of the ionphoric coccidiostats narasin , monensin, lasalocid and salinomycin in eggs by liquid chromatography/ tandem mass spectrometry[J].Wiley InterSci., 2005, 19: 533-539
[65] Cha J M, Yang S, CarLson K H. Rapid analysis of trace levels of antibiotic Polyether ionophores in surface water by solid-phase extraction and liquid chromatography with ion trap tandem mass spectrometric detection[J]. J. Chromatogr. A, 2005, 1065: 187-198
[66]Vincent U, Chedin M, Yasar S, et al. Determination of ionophore coccidiostats in feedingstuffs by liquid chromatography- tandem mass spectrometry part ?. Applcation to targeted feed[J]. J. Pharm. Bio. Anal., 2008, 47: 750-757
[67]Sparidans R W, Lagas J S, Schinkel A H. Liquid chromatography-tandem mass spectrometric assays for salinomycin in mouse plasma, liver, brain and small intestinal contents[J]. J. Chromatogr. B, 2007, 855: 200-210
[68]瞿永前,袁忠.抗莫能菌素多克隆抗体检测鸡组织中莫能菌素残留的研究[J].中国家禽, 2003, 25(20): 12-13
[69]Muldoon M T, Elissalde M H, Beier R C, et al. Development and validation of Monoclonal antibody-based enzyme-linked immunosorbent assay for salinomycin in chicken liver tissue[J]. J. Agric. Food Chem., 1995, 43: 1745-1750
[70]Peippo P, TuomoLa M, Lovgren T, et al. Rapid time-resolved fluoroimmunoassy for the screening of narasin and salinomycin residues in poultry and eggs[J]. J. Agric. Food Chem., 2004, 52(7): 1824-1828
[71]倪月菊.日本“肯定列表制度”的实施及其对我国食品和农产品的影响[J].国际贸易, 2006, 7: 22-25
[72]刘红卫,周围,高黎红,等.超高效液相色谱-串联四级杆质谱法测定肠衣中氯霉素残留量[J].中国兽药杂志, 2008, 42(2): 20-22
[73]刘志广.仪器分析学习指导与综合练习[M].高等教育出版社, 2005.9
[74]朱明华.仪器分析[ M].北京:高等教育出版社, 2000, 64-65
[75]徐葆筠,杨根元,金瑞祥等.实用仪器分析[M].北京:北京大学出版社, 1993. 193-194
[76]Veterinary Drugs Directorate of Canada. The Food and Drug Regulations: Monensin. Federal Register: 2004- 1-15:9450-5-11. http://www.hc-sc.gc.ca/dhp-mps/consultation /vet/consultations/past-anterieures/residu/mrl-lmr_monensin-eng.php
[77]Breckenrige, Colorado,United States of America.Joint FAO/WHO standards programme codex committee on residues of veterinary drugs in foods[s]. CX/RVDF 07/17/11,2007-9, ftp://ftp.fao.org/codex/ccrvdf17/rv17_11e.pdf
[78]European Medicines Agency, Veterinary Medicines and Inspection.Committee for Medicinal Products for Veterinary Use : Lasalocid Sodium[s]. 2006-7, EMEA/ CVMP/46049/2006-FINAL.http://www.emea.europa.eu/pdfs/vet/mrls/4604906en.pdf
[79]Elanco Products Data For Meat Export: U.S.– Japan[s] 2006,6,08,http:www.pork.org/ producers/docs/JapanMRL/Elanco/ElancoProductlisting.pdf
[80]陈明,陈美琴,耿志明,等.鸡蛋中聚醚类抗生素残留检测方法研究[J].中国食品学报,2006, 6(5): 124-125
[81]马立农,陈杖榴.高效液相色谱柱前衍生化法测定饲料中的盐霉素[J].中国兽药杂志, 2002, 36(2): 33-35
[82]Matabudul D K, Lumley I D, Points J S. The determination of 5 anticoccidial drugs (nicarbazin, lasalocid, monensin, salinomycin and narasin) in animal livers and eggs by liquid chromatography linked with tandem mass spectrometry(LC-MS-MS)[J]. Anal., 2002, 127(6): 760-768
[83]JAP-074角黄素检测方法, http://down.foodmate.net/standard/sort/13/10535.html
[84]农业部农药检定所.农药残留量实用检测方法手册(第一卷)[M].北京,中国农业科技出版社
[85]王立,汪正范.色谱分析样品处理(第二版)[M].北京,化学工业出版社. 2006
[86]周小锋,田晖.中国与欧盟农药残留状况标准比较研究[J].内蒙古农业科技, 2006, 2: 17-20
[87]朱俊杰,陆利霞,熊晓辉.食品中农残检测及预处理新技术进展[J].食品研究与开发, 2002, 29(2): 129-130
[88]于世林.高效液相色谱方法及应用[M].北京:化学工业出版社, 2001. 105～127
[89]呼世斌,李敬慈.分析化学[M].北京,世界图书出版公司, 1996
[2]佟恒敏,李艳华,韩建春.我国动物性食品中兽药残留的现状及为危害[J].黑龙江畜牧兽医,2003, 11, 61-62
[3]吕秀娟.降低畜禽药物残留的基本原则[J].兽药导刊, 2008, 7: 39-40
[4]胡登兵,丁新建,张焕容.兽药残留危害及国内外一般控制措施[J].四川畜牧兽医, 2008,河南畜牧兽医, 2003, 9(24): 21
[5]马艳梅.动物性食品兽药残留及控制措施[J] .江西畜牧兽医杂志, 2005, 1: 37-38
[6]贾久满,贾长江,石洪凌.动物性食品中抗生素残留对青少年儿童肥胖的影响[J].中华实用中西医杂志, 2004, 17(4): 1397-1398
[7]丁全福主编.药理学[M].北京:人民出版, 2001, 249-250
[8]李红,张莹蕾,李永军,马伟华.高效液相色谱法测定牛奶中氯霉素残留的研究综述[J].河南畜牧兽医, 2007, 28(2): 11
[9]吴祥集.动物性食品中兽药残留对人体健康的危害及其控制[J].贵州畜牧兽医, 2006, 30(3) : 25-27
[10]李娜.鸡组织中三种聚醚类抗生素残留的微生物法检测研究[D].安徽农业大学, 2007
[11]刘忠琛,张建波,管瑛,等.畜产品药物残留的危害及控制策略[J].广州饲料, 2004, 2(13): 9-11
[12]中华人民共和国农业部,关于发布《动物性食品中兽药最高残留限量》的通知, 1999-9-13, http://www.agri.gov.cn/xumugb/99-2-2.htm
[13]沈建忠,何继红.浅谈兽药残留分析技术研究进展[J].中国禽业导刊, 2004, 21: 15-16
[14]胡登兵,丁新建,张焕容.兽药残留危害及国内外一般控制措施[J].四川畜牧兽医, 2008,河南畜牧兽医, 2003, 9(24): 21
[15]欧盟抗生素残留仍然不可忽视[J] .中国动物保健, 2006, 6: 57
[16]张许科,刘兴金.国内外兽药发展趋势及对策[J] .中国家禽2004, 24(7): 1-4
[17] Kim S, Carlson K. Quantification of human and veterinary antibiotics in water and sediment using SPE/LC/MS/MS[J]. Anal. Bioanal. Chem., 2007, 387: 1301-1305
[18] Dimenna G P, Creegan J A, Turnbull L B. et al. Determination of Sodium salinomycin in chicken skin/fat by High-performance liquid chromatography utilizing column switching and UV detection[J]. J. Agric. Food Chem., 1986, 34(5): 805-810
[19] Elissalde M H, Beier R C, Rowe L D, et al. Development of a Monoclonal-based enzyme-linked immunosorbent assay for the coccidiostat salinomycin[J]. J. Agric. Food Chem., 1993, 41(11): 2167-2171
[20] Blanchflower W J, Kenndy D G. Determination of monensin, salinomycin and narasin in muscle, liver and eggs from domestic fowl using liquid chromatography-electrospray mass spectrometry[J]. J. Chromatogr. B, 1996, 675: 225-230
[21]商军,吴霞云,顾欣.莫能菌素微生物检定法的改进[J].中国兽药杂志, 1999, 33(1): 7-9
[22] Berger J, Rachlin A I, Scott W E, et al. The isolation of three crystalline antibiotics from Streptomyces[J]. J. Am. Chem. Soc., 1951, 73: 5295～5298
[23]Mallams A. K. Antibiotics(Polyethers)[J]. In Encyclopedia of Chemical Technology, Wiley: New York, 1978, 3: 47-63
[24]阎晓菊,顾觉奋.聚(多)醚类抗生素(综述) [J].现代应用药学, 1987, 4(4): 43-46
[25]杨桂香,曾振灵,陈杖榴.聚醚类抗生素对肉鸡的毒性作用及其合理应用[J].养禽与禽病防治, 2001, 2: 13-14
[26]吕爱军,穆阿丽,宋小敬,等.聚醚类抗生素的作用机理及应用研究进展[J].吉林畜牧兽医. 2004, 5: 22-24
[27]倪月菊.日本“肯定列表制度”的实施及其对我国食品和农产品的影响[J].国际贸易, 2006, 7: 22-25
[28]陈明,耿志明,王冉,等.饲料中聚醚类抗生素的柱后衍生同时测定方法研究[J].中国饲料,2005, 20: 27-29
[29]Martin D R, Rowley L, Shearer G, et al. Effect of cooking on Veterinary drug residues in food. 6. Lasalocid[J]. J. Agric. Food Chem., 1997, 45(3): 927
[30]李娜,祁克宗,朱良强等.聚醚类抗生素残留检测方法的研究进展[J].家禽科学,2007,5:38-40
[31]霍晓荣,刘铁铮,王冉,等.盐霉素和莫能菌素残留分析方法的研究进展[J].中国畜牧兽医, 2005, 32(7): 23-24
[32]肖琳,黄为一.尼日利亚菌素高产菌株的选育[J].微生物学通报, 2002, 29(4): 59
[33]罗洁,谢天尧,刘秋英,等.聚醚类抗生素盐霉素的毛细管电泳-电导分离检测研究[C] .第三届全国微全分析系统学术会议论文集, 2005, 10: 246-247
[34] Miyazaki Y, Shibuya M, Sugawara H, et al. Salinomycin, a new Polyether antibiotic[J]. J. Antibiot, 1974, 11: 814-821
[35]李启琳,李燕鹏,王士长.鸡肉中残留盐霉素的高效液相色谱检测法[J].农产品加工, 2007, 10: 67-68
[36]沈建忠,钱传范,杨汉春,等.马杜霉素在鸡组织中残留检测方法的研究[J].畜牧兽医学报, 1999, 30(2) :172-179
[37]周伟伟,卜仕金.聚醚类离子载体抗生素的研究进展[J].兽药与饲料添加剂, 2006, 11(3) :13-15
[38]杨桂香,陈杖榴.聚醚类抗生素毒性研究进展[J] .动物医学进展, 2000, 2( 4) : 2-5
[39] Badiola J J, Luco D F, Perz M A, et al. Mauduramycin and tiamulin compatibility in broiler chickens[J]. Avian Patho., 1994, 23: 3-17
[40]马学海,施玉樑.离子载运体的大家族-多醚类抗生素[J].生物学通报,1996,31(6):1-3
[41]朱模忠.兽药手册[M]. 1版.北京:化工出版社, 2002: 194-197
[42]刘继业,苏晓欧.饲料安全工作手册[M].北京:中国农业出版社, 2001: 17-40
[43]张丹红,王恩,周元林.莫能菌素中毒致横纹肌溶解症三例[J].中华神经科杂志,2006, 39(2) : 88
[44]刘燕,高萍.莫能菌素中毒致多器官功能障碍4例的护理体会[J]. 2005, 31 (6): 430-431
[45]潘蕴慈,董金芝,边景荣,等.盐霉素对肉鸡残留量的测定[J].科学试验与研究, 1992, 9: 8-9
[46]Cabadaj R, Nagy J, Popelka P, et al. The determination of Salinomycin residues in the tissues of broiler chickens by using microbiological diffusion methods[J]. Slove. Vet. Res., 2002, 39 (2): 137-143
[47]Kozarova I, Mate D, Cabadaj R et al. An evaluation of the microbiological diffusion methods as a tool for screening monensin residues in the tissues of broiler chickens[J]. Folia Vet., 2002,46(1): 27-33
[48]李俊锁,邱月明,王超.兽药残留分析[M].上海:上海科技出版社, 2002:538-550
[49]国家药典委员会.中华人民共和国药典(二部,附录Ⅺ)[M].北京化学工业出版社,2005: 22-24
[50]Golab T, Barton S J, Scroggs R E. Colorimetric method for monensin[J]. J. Assoc. Off Anal. Chem., 1973, 56(1): 171-173
[51]Owles P J. Identification of monensin, narasin, salinomycin and lasalocid in pre-mixes and feeds by thin-layer chromatography[J]. Anal., 1984, 109(10):1331-1333
[52]Landgraf W W, Ross F P. Thin-layer chromatographic determination of monensin in feeds: screening method[J]. J. AOAC Int, 1998, 81(4): 844-847
[53]陈运勤,李跃龙,伍绍登,等.用薄层扫描法测定马杜霉素残留[J].中国动物保健, 2003, 7: 21-23
[54]Martinez E E, Shimoda W. Identification and semiquantitation of monensin sodium in animal feeds by thin layer bioautography[J]. J. Assoc. Off Anal. Chem., 1983, 66(6): 1506-1509
[55]VanderKop P A, MacNeil J D. Separation and detection of monensin, salinomycin and lasalocid in animal feeds by thin layer bioautography[J]. J. Chromatogr. A, 1990, 508(2): 386-390
[56]农业部.动物源食品中莫能菌素和盐霉素残留检测方法-高效液相色谱法[J].中国兽药杂志, 2002, 36(8): 9-10
[57]张素霞,沈建忠,吕亚滨,等.莫能菌素和盐霉素在鸡组织中的残留分析方法研究[J].畜牧兽医学报, 2000, 31(6): 530-535
[58]陈笑梅,施旭霞.柱后衍生高效液相色谱法测定鸡肉中莫能菌素残留量[J].色谱, 1999, 17(1): 77-79
[59]项新华,涂晓明,贾明宏,等.高效液相色谱法检测动物组织中马杜霉素残留[J].中国公共卫生, 2002, 18(1): 101-102
[60]Blanchflower W J, Rice D A, HamiLton J T. Simultaneous high-performance liquid chromatographic determination of monensin, narasin and salinomycin in feeds using post-column derivatisation[J]. Anal., 1985, 110(11): 1283-1287
[61]Dusi G, Gamba V. Liquid chromatography with ultraviolet detection of lasalocid , monensin, salinomycin and narasin in poultry using pre-column derivatization[J]. J. Chromatogr. A, 1999, 835: 243-246
[62]Hormazábal V, Yndestad M. Ostensvik O.Determination of amprolium, ethopabate, lasalocid, monensin, narasin and salinomycin in chicken tissues, plasma, and egg using liquid chromatography-mass spectrometry[J]. Liqu. Chromatogr. Related Tech., 2002, 23(10): 585-1598
[63]Heller D N, Nochetto C B. Development of multiclass methods for drug residues in eggs: silica SPE cleanup and LC-MS/MS analysis of lonophore and macrolode residues[J]. J. Agric. Food Chem., 2004, 52(23): 6848-6856
[64]Mortier L, Daeseleire E, Peteghem C V. Determination of the ionphoric coccidiostats narasin , monensin, lasalocid and salinomycin in eggs by liquid chromatography/ tandem mass spectrometry[J].Wiley InterSci., 2005, 19: 533-539
[65] Cha J M, Yang S, CarLson K H. Rapid analysis of trace levels of antibiotic Polyether ionophores in surface water by solid-phase extraction and liquid chromatography with ion trap tandem mass spectrometric detection[J]. J. Chromatogr. A, 2005, 1065: 187-198
[66]Vincent U, Chedin M, Yasar S, et al. Determination of ionophore coccidiostats in feedingstuffs by liquid chromatography- tandem mass spectrometry part ?. Applcation to targeted feed[J]. J. Pharm. Bio. Anal., 2008, 47: 750-757
[67]Sparidans R W, Lagas J S, Schinkel A H. Liquid chromatography-tandem mass spectrometric assays for salinomycin in mouse plasma, liver, brain and small intestinal contents[J]. J. Chromatogr. B, 2007, 855: 200-210
[68]瞿永前,袁忠.抗莫能菌素多克隆抗体检测鸡组织中莫能菌素残留的研究[J].中国家禽, 2003, 25(20): 12-13
[69]Muldoon M T, Elissalde M H, Beier R C, et al. Development and validation of Monoclonal antibody-based enzyme-linked immunosorbent assay for salinomycin in chicken liver tissue[J]. J. Agric. Food Chem., 1995, 43: 1745-1750
[70]Peippo P, TuomoLa M, Lovgren T, et al. Rapid time-resolved fluoroimmunoassy for the screening of narasin and salinomycin residues in poultry and eggs[J]. J. Agric. Food Chem., 2004, 52(7): 1824-1828
[71]倪月菊.日本“肯定列表制度”的实施及其对我国食品和农产品的影响[J].国际贸易, 2006, 7: 22-25
[72]刘红卫,周围,高黎红,等.超高效液相色谱-串联四级杆质谱法测定肠衣中氯霉素残留量[J].中国兽药杂志, 2008, 42(2): 20-22
[73]刘志广.仪器分析学习指导与综合练习[M].高等教育出版社, 2005.9
[74]朱明华.仪器分析[ M].北京:高等教育出版社, 2000, 64-65
[75]徐葆筠,杨根元,金瑞祥等.实用仪器分析[M].北京:北京大学出版社, 1993. 193-194
[76]Veterinary Drugs Directorate of Canada. The Food and Drug Regulations: Monensin. Federal Register: 2004- 1-15:9450-5-11. http://www.hc-sc.gc.ca/dhp-mps/consultation /vet/consultations/past-anterieures/residu/mrl-lmr_monensin-eng.php
[77]Breckenrige, Colorado,United States of America.Joint FAO/WHO standards programme codex committee on residues of veterinary drugs in foods[s]. CX/RVDF 07/17/11,2007-9, ftp://ftp.fao.org/codex/ccrvdf17/rv17_11e.pdf
[78]European Medicines Agency, Veterinary Medicines and Inspection.Committee for Medicinal Products for Veterinary Use : Lasalocid Sodium[s]. 2006-7, EMEA/ CVMP/46049/2006-FINAL.http://www.emea.europa.eu/pdfs/vet/mrls/4604906en.pdf
[79]Elanco Products Data For Meat Export: U.S.– Japan[s] 2006,6,08,http:www.pork.org/ producers/docs/JapanMRL/Elanco/ElancoProductlisting.pdf
[80]陈明,陈美琴,耿志明,等.鸡蛋中聚醚类抗生素残留检测方法研究[J].中国食品学报,2006, 6(5): 124-125
[81]马立农,陈杖榴.高效液相色谱柱前衍生化法测定饲料中的盐霉素[J].中国兽药杂志, 2002, 36(2): 33-35
[82]Matabudul D K, Lumley I D, Points J S. The determination of 5 anticoccidial drugs (nicarbazin, lasalocid, monensin, salinomycin and narasin) in animal livers and eggs by liquid chromatography linked with tandem mass spectrometry(LC-MS-MS)[J]. Anal., 2002, 127(6): 760-768
[83]JAP-074角黄素检测方法, http://down.foodmate.net/standard/sort/13/10535.html
[84]农业部农药检定所.农药残留量实用检测方法手册(第一卷)[M].北京,中国农业科技出版社
[85]王立,汪正范.色谱分析样品处理(第二版)[M].北京,化学工业出版社. 2006
[86]周小锋,田晖.中国与欧盟农药残留状况标准比较研究[J].内蒙古农业科技, 2006, 2: 17-20
[87]朱俊杰,陆利霞,熊晓辉.食品中农残检测及预处理新技术进展[J].食品研究与开发, 2002, 29(2): 129-130
[88]于世林.高效液相色谱方法及应用[M].北京:化学工业出版社, 2001. 105～127
[89]呼世斌,李敬慈.分析化学[M].北京,世界图书出版公司, 1996