动物性食品中大环内酯类和林可胺类多残留定量与确证方法研究
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摘要
大环内酯类药物是一类广泛使用的药物,可分为大环内酯类抗生素和大环内酯抗寄生虫(阿维菌素类)两类。大环内酯抗生素在兽医上广泛用于治疗牛、羊、猪、禽的呼吸道疾病和肠道细菌感染,也用于饲料添加剂以促进动物生长。大环内酯抗寄生虫已经在世界范围内用于保障人、动物和植物的健康,它可以杀灭寄生虫,如蛔虫、肺虫和螨虫等。
在兽医治疗上,抗生素联合用药非常普遍。联合用药可以带来单独使用所没有的效果,林可霉素、壮观霉素复方制剂(比率1:2)就是其中一例。壮观霉素、林可霉素两者联合使用具协同作用,常用于治疗生长期家禽的慢性呼吸道疾病、支原体肺炎和腹泻等。
这些抗生素药物的不正确使用会在可食性组织中残留,对消费者产生毒性反应,如过敏人群会产生过敏反应,或诱导耐药菌株产生而引起间接危害。阿维菌素类毒性低,但其在动物体内残留时间长,可能会对人体造成危害。关于这些药物的多残留方法,国内外虽有报道,但目前还没有不同种类药物的多残留方法,并且检测种类也较少。因此本研究从建立不同种类药物的多残留方法展开研究,建立了大环内酯类抗生素和大环内酯抗寄生虫、林可胺和壮观霉素两个多残留方法,以监测这些药物在动物可食性组织的残留。
方法一是建立动物可食性组织中大环内酯类药物的HPLC-MS/MS法。组织样品用甲醇/乙腈(1:1)混合溶液提取,正己烷脱脂,40℃水浴下缓慢蒸干提取液。残余物甲醇溶解,40℃水浴下氮气缓慢吹干,流动相0.5mL溶解,12,000rpm离心后取10μL进样。检测采用选择反应监测(SRM)模式。结果表明,大环内酯类在组织中的检出限(CCα;α1%)在0.3μg/kg～1.5μg/kg之间,定量限(CCβ;β5%)在0.5μg/kg～2.5μg/kg之间。在不同加标水平下,平均回收率在64.3%～88.0%之间,日间变异系数在4.6%～24.3%之间。
方法二是以固相萃取和衍生为基础,建立同时检测猪、牛、鸡可食性组织以及鸡蛋和牛奶中林可霉素、壮观霉素的气相色谱分析法和林可霉素、克林霉素和壮观霉素的气质确证方法。组织样品用磷酸缓冲液/三氯乙酸混合液提取,加入离子对试剂,供SPE净化,甲醇洗脱,洗脱液40℃水浴氮气吹干。残余物加乙腈和BSTFA于75℃反应60min,用氮气缓慢吹干,正己烷定容,离心,取1μL上清液用气相色谱和气相色谱-质谱联用测定。
气相色谱定量方法结果显示,组织中林可霉素和壮观霉素的最低检测限分别是20μg/kg、30μg/kg,最低定量限分别是30μg/kg、40μg/kg。在四个加标水平下,林可霉素和壮观霉素回收率介于70.6%～86.5%之间,日间变异系数≤12.6%。
确证方法以选择离子监测(SIM)为测定方法。林可霉素和克林霉素均以离子126为定量离子,壮观霉素以145为定量离子。该条件下,林可霉素的最低检测限和最低定量限分别是3μg/kg和5μg/kg,克林霉素的最低检测限和最低定量限分别是15μg/kg和20μg/kg,壮观霉素的最低检测限和最低定量限分别是15μg/kg和20μg/kg。平均回收率介于68.3%～85.2%之间,变异系数≤15.1%。
本课题通过对样品前处理及色谱、质谱条件的大量优化,建立的两个方法均为同时检测不同类药物的多残留方法。方法新颖,在国内外处于领先地位,极具创新性。方法的建立为加强这些药物的监控提供了技术保障,有利于增加出口创汇、保证国际之间正常贸易往来、保障人类健康,具有十分重要的意义和实用价值。
Macrolides are a large class of drugs used widely,which can be divided into two diverse,macrolide antibiotics and macrocyclic lactones.Macrolide antibiotics are widely used in veterinary medicine to treat respiratory diseases and enteric infections in cattle, sheep,swine and poultry.However,they are also employed as feed additives to promote animal growth.Macrocyclic lactones(MLs) have found widespread application in hunman and animal health and crop protection,and are used to combat parasitic infection,such as roundworms,lungworms and mites.
In veterinary treatment,combination of antibiotics from different group is very popular. Combination can result in better effect than one be used separately,as it did in the case of Lincomycin Hydrochloride and Spectinomycin Sulfate Premix(in a ratio 1:2).The combination can prevent and treat chronic respiratory of respiratory disease of growing poultry,mycoplasmal infections or dysentery.
Incorrect use of these antibiotics may leave residues in edible tissues causing toxic effect on consumers,e.g.allergic reactions in hypersensitive individuals,or indirectly, problems through the induction of resistant strains of bacteria.Macrocyclic lactones are low-toxins,but the presence of residues may affect consumer health.Many muti-resisues methods about these drugs have been reported,but they can not determinate different class simutanously and analyse only several.Therefore,simple and reliable analytic methods are required to monitor these drug residues in the edible tissues of livestock animals.
The first method is to determinate macrolides in edible tissues by HPLC-MS/MS.The samples were extracted with mixture of metheanol and acetonitrile(1:1).Then the extract was defatted with hexane and evaporated to nearly dryness at 40℃.The residue was dissolved in metheanol and evaporated to dryness under a stream of nitrogen.Then the residues was dissolved with mobile-phase and centrifuged in 12000rpm,10μL of which was injected into HPLC-MS/MS.Determination was performed in SRM mode.The experiment indicated that,an averaged decision limits(CCα;α1%) and detection capability(CCβ;β5%) of the method were in the range of 0.3μg/kg～1.5μg/kg and 0.5μg/kg～2.5μg/kg in the tissues,respectively.The average recoveries of different fortified samples of Marolides were in the range of 64.3%～88.0%;the average standard derivations were in the range of 4.6%～24.3%.
The second method is based on solide-phase extraction and pre-derivatized,which can determinate Lincomycin and Spectinomycin in several tissues by GC and confirme Lincomycin,Clindamycin and Spectinomycin by GC-MS.The samples were extracted with phosphate buffer and cleaned up with C_(18) solid-phase extraction(SPE).The cartridge was eluted with 4 ml of methanol and the eluate was evaporated to dryness in a stream of nitrogen at 40℃.Then acetonitrile and BSTFA were added to the tube and the mixture reacted at 75℃for 60 min.The raimnant was evaporated to complete dryness with a stream of nitrogen.The residue was dissolved in hexane,1ul of which was injected into GC or GC-MS.
The quantitative methed indicated that,LOD and LOQ of Lincomycin in tissues is 20μg/kg and 30μg/kg,of Spectinomycin is 30μg/kg and 40μg/kg.The average recoveries of four different fortified samples of Lincomycin and Spectinomycin were in the range of 70.6%～86.5%;the average standard derivations was below 12.6%.
The confirmation method was based on the SIM mode.The quanitative ions for Lincomycin,Clindamycin and Spectinomycin were 126,126 and 145,respectively.Under this condition,the LOD for Lincomycin,Clindamycin and Spectinomycin were 3μg/kg, 15μg/kg and 15μg/kg,respectively;the LOQ for Lincomycin Clindamycin and Spectinomycin were 5μg/kg,20μg/kg and 20μg/kg.The average recoveries were in the range of 68.3%～85.2%and the average standard derivations were below 15.1%.
The conditions of sample preparation and detection by chromatography and mass-spectrometer were optimized in this study.These two methods were to simultaneously determinate the residues of drugs from different class.The methods were new and in the frontiers of residue analysis.The deveiopment of the methods provide technical support for monitoring of residues of these drugs in food derived from Animals.
在兽医治疗上,抗生素联合用药非常普遍。联合用药可以带来单独使用所没有的效果,林可霉素、壮观霉素复方制剂(比率1:2)就是其中一例。壮观霉素、林可霉素两者联合使用具协同作用,常用于治疗生长期家禽的慢性呼吸道疾病、支原体肺炎和腹泻等。
这些抗生素药物的不正确使用会在可食性组织中残留,对消费者产生毒性反应,如过敏人群会产生过敏反应,或诱导耐药菌株产生而引起间接危害。阿维菌素类毒性低,但其在动物体内残留时间长,可能会对人体造成危害。关于这些药物的多残留方法,国内外虽有报道,但目前还没有不同种类药物的多残留方法,并且检测种类也较少。因此本研究从建立不同种类药物的多残留方法展开研究,建立了大环内酯类抗生素和大环内酯抗寄生虫、林可胺和壮观霉素两个多残留方法,以监测这些药物在动物可食性组织的残留。
方法一是建立动物可食性组织中大环内酯类药物的HPLC-MS/MS法。组织样品用甲醇/乙腈(1:1)混合溶液提取,正己烷脱脂,40℃水浴下缓慢蒸干提取液。残余物甲醇溶解,40℃水浴下氮气缓慢吹干,流动相0.5mL溶解,12,000rpm离心后取10μL进样。检测采用选择反应监测(SRM)模式。结果表明,大环内酯类在组织中的检出限(CCα;α1%)在0.3μg/kg～1.5μg/kg之间,定量限(CCβ;β5%)在0.5μg/kg～2.5μg/kg之间。在不同加标水平下,平均回收率在64.3%～88.0%之间,日间变异系数在4.6%～24.3%之间。
方法二是以固相萃取和衍生为基础,建立同时检测猪、牛、鸡可食性组织以及鸡蛋和牛奶中林可霉素、壮观霉素的气相色谱分析法和林可霉素、克林霉素和壮观霉素的气质确证方法。组织样品用磷酸缓冲液/三氯乙酸混合液提取,加入离子对试剂,供SPE净化,甲醇洗脱,洗脱液40℃水浴氮气吹干。残余物加乙腈和BSTFA于75℃反应60min,用氮气缓慢吹干,正己烷定容,离心,取1μL上清液用气相色谱和气相色谱-质谱联用测定。
气相色谱定量方法结果显示,组织中林可霉素和壮观霉素的最低检测限分别是20μg/kg、30μg/kg,最低定量限分别是30μg/kg、40μg/kg。在四个加标水平下,林可霉素和壮观霉素回收率介于70.6%～86.5%之间,日间变异系数≤12.6%。
确证方法以选择离子监测(SIM)为测定方法。林可霉素和克林霉素均以离子126为定量离子,壮观霉素以145为定量离子。该条件下,林可霉素的最低检测限和最低定量限分别是3μg/kg和5μg/kg,克林霉素的最低检测限和最低定量限分别是15μg/kg和20μg/kg,壮观霉素的最低检测限和最低定量限分别是15μg/kg和20μg/kg。平均回收率介于68.3%～85.2%之间,变异系数≤15.1%。
本课题通过对样品前处理及色谱、质谱条件的大量优化,建立的两个方法均为同时检测不同类药物的多残留方法。方法新颖,在国内外处于领先地位,极具创新性。方法的建立为加强这些药物的监控提供了技术保障,有利于增加出口创汇、保证国际之间正常贸易往来、保障人类健康,具有十分重要的意义和实用价值。
Macrolides are a large class of drugs used widely,which can be divided into two diverse,macrolide antibiotics and macrocyclic lactones.Macrolide antibiotics are widely used in veterinary medicine to treat respiratory diseases and enteric infections in cattle, sheep,swine and poultry.However,they are also employed as feed additives to promote animal growth.Macrocyclic lactones(MLs) have found widespread application in hunman and animal health and crop protection,and are used to combat parasitic infection,such as roundworms,lungworms and mites.
In veterinary treatment,combination of antibiotics from different group is very popular. Combination can result in better effect than one be used separately,as it did in the case of Lincomycin Hydrochloride and Spectinomycin Sulfate Premix(in a ratio 1:2).The combination can prevent and treat chronic respiratory of respiratory disease of growing poultry,mycoplasmal infections or dysentery.
Incorrect use of these antibiotics may leave residues in edible tissues causing toxic effect on consumers,e.g.allergic reactions in hypersensitive individuals,or indirectly, problems through the induction of resistant strains of bacteria.Macrocyclic lactones are low-toxins,but the presence of residues may affect consumer health.Many muti-resisues methods about these drugs have been reported,but they can not determinate different class simutanously and analyse only several.Therefore,simple and reliable analytic methods are required to monitor these drug residues in the edible tissues of livestock animals.
The first method is to determinate macrolides in edible tissues by HPLC-MS/MS.The samples were extracted with mixture of metheanol and acetonitrile(1:1).Then the extract was defatted with hexane and evaporated to nearly dryness at 40℃.The residue was dissolved in metheanol and evaporated to dryness under a stream of nitrogen.Then the residues was dissolved with mobile-phase and centrifuged in 12000rpm,10μL of which was injected into HPLC-MS/MS.Determination was performed in SRM mode.The experiment indicated that,an averaged decision limits(CCα;α1%) and detection capability(CCβ;β5%) of the method were in the range of 0.3μg/kg～1.5μg/kg and 0.5μg/kg～2.5μg/kg in the tissues,respectively.The average recoveries of different fortified samples of Marolides were in the range of 64.3%～88.0%;the average standard derivations were in the range of 4.6%～24.3%.
The second method is based on solide-phase extraction and pre-derivatized,which can determinate Lincomycin and Spectinomycin in several tissues by GC and confirme Lincomycin,Clindamycin and Spectinomycin by GC-MS.The samples were extracted with phosphate buffer and cleaned up with C_(18) solid-phase extraction(SPE).The cartridge was eluted with 4 ml of methanol and the eluate was evaporated to dryness in a stream of nitrogen at 40℃.Then acetonitrile and BSTFA were added to the tube and the mixture reacted at 75℃for 60 min.The raimnant was evaporated to complete dryness with a stream of nitrogen.The residue was dissolved in hexane,1ul of which was injected into GC or GC-MS.
The quantitative methed indicated that,LOD and LOQ of Lincomycin in tissues is 20μg/kg and 30μg/kg,of Spectinomycin is 30μg/kg and 40μg/kg.The average recoveries of four different fortified samples of Lincomycin and Spectinomycin were in the range of 70.6%～86.5%;the average standard derivations was below 12.6%.
The confirmation method was based on the SIM mode.The quanitative ions for Lincomycin,Clindamycin and Spectinomycin were 126,126 and 145,respectively.Under this condition,the LOD for Lincomycin,Clindamycin and Spectinomycin were 3μg/kg, 15μg/kg and 15μg/kg,respectively;the LOQ for Lincomycin Clindamycin and Spectinomycin were 5μg/kg,20μg/kg and 20μg/kg.The average recoveries were in the range of 68.3%～85.2%and the average standard derivations were below 15.1%.
The conditions of sample preparation and detection by chromatography and mass-spectrometer were optimized in this study.These two methods were to simultaneously determinate the residues of drugs from different class.The methods were new and in the frontiers of residue analysis.The deveiopment of the methods provide technical support for monitoring of residues of these drugs in food derived from Animals.
引文
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48. Delia W M, Yiu C W, Alec C B. Quantitative analysis of lincomycin in animal tissue and bovine milk by liquid chromatography electrospray ionization tandem mass spectrometry. Journal of Pharmaceutical Biomedical Analysis, 2004, 34: 651-659
49. Dolan J W. Improving an ion-pairing method. LC GC, 1996, 14: 768
50. Dousa M, Sikac Z, Halama M, Lemr K. HPLC determination of lincomycin in premixes and feedstuffs with solid-phase extraction on OASIS HLB and LC-MS/MS confirmation. Journal of Pharmaceutical Biomedical Analysis, 2006, 40(4): 981-986
51. Draisci R, delli Quadri F, Achene L, Volpe G, Palleschi L, Palleschi L. A new electrochemical enzyme-linked immunosorbent assay for the screening of macrolide antibiotic residues in bovine meat. Analyst, 2001, 126(11): 1942
52. Dubois M, Fluchard D, Sior E, Delahaut P. Identification and quantification of five macrolide antibiotics in several tissues, eggs and milk by liquid chromatography- electrospray tandem mass spectrometry. Journal of Chromatography B: Biomedical Sciences and Applications, 2001, 753(2): 189-202
53. Elrod L Jr, Bauer J F, Messner S L. Determination of spectinomycin dihydrochloride by liquid chromatography with electrochemical detection. Pharmaceutical research, 1998, 10(5): 664-667
54. Farrington W H, Cass S D, Patey A L, Shearer G. A method for the analysis of lincomycin in porcine and bovine kidney. Food Additives & Contaminants, 1988, 5 (1): 67-75
55. Fink D W, DeMontigny P, Shim J S K. Evolution of a specific fluorogenic derivatization of ivermectin for bioanalytical applications. Analyst, 1996,121: 1533
56. Gonzalez de la, Huebra M J, Bordin G, Rodriguez A R. A multiresidue method for the simultaneous determination of ten macrolide antibiotics in human urine based on gradient elution liquid chromatography coupled to coulometric detection (HPLC-ECD). Analytica Chimica Acta, 2004, 517: 53
57. Gusev, Isabelle, Huang, Xian, Horvath, Csaba Capillary with columns in situformed porous monolithic packing for micro high-performance liquid chromatography and capillary electrochromatography. Journal of Chromatography A, 1999, 855(1): 273-290
58. Haagsma N, Keegstra J R, Scherpenisse P. High-performance liquid chromatographic determination of spectinomycin in swine, calf and chicken plasma. Journal of Chromatography, 1993, 615(2): 289-295
59. Haagsma N, Scherpenisse P, Simmonds RJ, Wood S A, Rees S A. High-performance liquid chromatographic determination of spectinomycin in swine, calf and chicken plasma using post-column derivatization. Journal of Chromatography B: Biomedical Sciences and Applications. 1995,672(1): 165-171
60. Hamamoto K, Mizuno Y, Koike R, Yamaoka R, Takahashi T, Takahashi Y. Residue analysis of spectinomycin in tissues of chicken and swine by HPLC. Shokuhin Eiseigaku Zasshi, 2003,44 (2): 114-118
61. Horie M, Saito K, Ishii R, Yoshida T, Haramaki Y, Nakazaw H. Simultaneous determination of five macrolide antibiotics in meat by high-performance liquid chromatography. Journal of Chromatography A, 812(1998): 295-302
62. Horie M, Takegami H, Toya K, Kikuchi Y, Nakazawa H. Determination of spiramycin and tilmicosin in meat and fish by LC/MS. Shokuhin Eiseigaku Zasshi, 2003, 44(3): 150-154
63. Hornish R E, Wiest J R. Quantitation of spectinomycin residues in bovine tissues by ion-exchange high-performance liquid chromatography with post-column derivatization and confirmation by reversed-phase high-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry. Journal of Chromatography A. 1998, 812(1-2): 123-133
64. Howells L, Sauer M J. Multi-residue analysis of avermectins and moxidectin by ion-trap LC-MS". Analyst, 2001,126: 155
65. Kawai J, Yamamoto T, Tohno S, Kitajima Y. Spectrochim Acta B, 1999, 1: 241
66. Kees F, Spangler S, Wellenhofer M. Determination of macrolides in biological matrices by high-performance liquid chromatography with electrochemical detection. Journal of Chromatography, 1998, 812: 287
67. Knox J H, Grant I H. J Chromatographia, 1991, 32: 317
68. Kwok D, Chow, P, Mori, B, Yong, M. A multi-residue ESI LC/MS/MS method for the determination of six aminoglycoside antimicrobial residues in fluid milk and animal tissues. 45th ASMS Conference on Mass Spectrometry, Palm Springs, CA, 1997, p. 960
69. Leal C, Codony R, Compano R, Granados M, Prat M D. Determination of macrolide antibiotics by liquid chromatography. Journal of Chromatography A, 2001, 910:285
70. Leroy P, Decolin D, Nicolas A. Determination of josamycin residues in porcine tissues using high-performance liquid chromatography with pre-column derivatization and spectrofluorime tric detection. Analyst, 1994, 119: 2743
71. Li J, Qian C. Determination of avermectinB_1 in biological samples immunoafinity colu- mn cleanup and liquid chromatography with UV detection. Journal of AOAC International, 1996, 79(5): 1062-1067
72. Luo W, Hansen E B, Ang C Y, Thompson H C. Determination of lincomycin residue in salmon tissues by ion-pair reversed-phase liquid chromatography with electrochemical detection. Journal of AOAC International, 1996, 79(4): 839-843
73. Marin S R, Olave S G., Andonie O E, Arlegui O G. International Journal of Environment Analytical Chemistry, 1993, 52: 127
74. Masakazu H, Harumi T, Kazuo T. Determination of macrolide antibiotics in meat and fish by liquid chromatography-electrospry mass spectrometry. Analytica Chimica Acta, 2003, 492(1-2): 187-197
75. Masakazu H, Harumi T, Kazuo T, Hiroyuki N. Determination of macrolide antibiotics in meat and fish by liquid chromatography electrospray mass spectrometry. Analytica Chimica Acta, 492(2003): 187-197
76. Matisova, E, Domotorova M. Fast gas chromatography and its use in trace analysis. Journal of Chromatography A, 2003, 1000(1-2): 199-221
77. Matsumoto E, Simabuco S M, Perez C A, Nascimento V F. X-raySpectrom, 2002, 2: 136.
78. McLaughlin L G, Henion J D. Determination of aminoglycoside antibiotics by reversed-phase ion-pairing high-performance liquid chromatography coupled with pulsed amperometry and ion spray mass spectrometry. Journal of Chromatography, 1992,591(1-2): 195
79. McLaughlin L G, Henion J D, Kijak P J. Multi-residue confirmation of aminoglycoside antibiotics and bovine kidney by ion spray high-performance liquid chromatography tandem mass spectrometry. Biological Mass Spectrometry, 1994, 23(7): 417-429
80. Mcmurray C H, Blanchflower W J, Rice D A. Gas chromatographic mass spectrometric detection and quantitation of lincomycin in animal feedingstuff. Journal of AO AC International, 1984, 67(3): 582-588
81. McNaught A D, Wilkinson A. Compendium of Chemical Terminology: The Gold Book (seconded). Blackwell Science, London, UK, 1997
82. Nagata T, Miyamoto F, Hasegawa Y, Ashizawa E. Simultaneous determination of residual antiparasitic lactones in bovine muscle and liver by liquid chromato- gramphy with fluorescence detection. Journal of AOAC International, 2003, 86(3): 490
83. Nakashima R, Kitagawa S, Yoshida T, Tsuda T. Study of flow rate in pressurized gradient capillary electrochromatography using splitter and separation of peptides using an Amide stationary phase. Journal of Chromatography A, 2004, 1044(1-2): 305-309
84. NdungOu K, Franks R P, Bruland K W, Flegal A R. Analytica Chimica Acta, 2003 481: 127
85. Pereira T, Chang S W. Semi-automated quantification of ivermectin in rat and human plasma using protein precipitation and filtration with liquid chromatogram- phy/tandem mass spectrometry. Rapid Communications in Mass Spectrometry, 2004, 18:1265
86. Peru K M, Kuchta S L, Headley J V, Cessna A J. Development of a hydrophilic interaction chromatography-mass spectrometry assay for spectinomycin and lincomycin in liquid hog manure supernatant and run-off from cropland. Journal of Chromatography A, 2006,1107(1-2): 152-158
87. Pollmeier M, Maier S, Moriarty K, Demontigny P. High-performance liquid chromato- graphic assay for the determination of a semisynthetic avermectin analog (eprinomectin) in bovine milk at parts per billion levels-method development and validation. Journal of Chromatography B, 2002, 772(1): 99-105
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