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1.
《中国家禽》2020,(8)
为有效检测鸡蛋中甲硝唑、诺氟沙星、强力霉素、氧氟沙星、培氟沙星、金刚烷胺、恩诺沙星、氟苯尼考、氯霉素9种药物残留,建立高效液相色谱-串联质谱(HPLC-MS/MS)分析方法,对方法中的提取液、仪器条件等进行优化;设计试验方案,考察方法的回收率、灵敏度及精密度。鸡蛋样品去壳混匀后用80%乙腈水溶液提取,PRiME HLB小柱净化,洗脱液经氮气吹干后用10%甲醇水溶液复溶,经0.22μm微孔滤膜过滤后,用高效液相色谱-串联质谱仪测定。分析方法采用电喷雾电离正负离子同时进行扫描,多反应监测(MRM)模式进行测定。在4个不同浓度的水平下,平均回收率在75.7%～95.7%;相对标准偏差(RSD)均小于10%;检测限(LOD,S/N3)和定量限(LOQ,S/N10)分别为1.0μg/kg和2.0μg/kg。本检测方法简便快捷,精确灵敏,稳定可靠,适用于对鸡蛋中多种药物残留的快速检测和分析。 相似文献
2.
建立了鸡蛋中氟虫腈及其代谢物残留的液相色谱/串联质谱检测方法分析方法。样品经乙腈提取,PRIME HLB净化脂肪,采用电喷雾离子源负离子检测模式(ESI-)和多重反应监测(MRM)模式测定,外标法定量分析。结果表明：氟虫腈及其代谢物在0.1～20 ng/mL的范围内均具有良好的线性关系,相关系数（R2）不小于0.9997,在2、10和20μg/kg不同加标浓度下的平均加标回收率为99.92%～108.3%,相对标准偏差：1.96%～5.01%,方法检出限为0.008～0.023μg/kg。该方法快速、简便、灵敏,适用于鸡蛋中氟虫腈及其代谢物的快速测定。 相似文献
3.
《中国家禽》2021,(11)
为高效检测鸡蛋中多种药物的残留,研究建立了能同时检测鸡蛋中硝基咪唑类、林可胺类、磺胺类、抗病毒类、大环内酯类、喹诺酮类、糖皮质激素类、喹乙醇类代谢物等8类76种药物的超高效液相色谱-串联质谱法(UPLC-MS/MS)。试验通过将鸡蛋样品去壳混匀后用0.2%(v/v)甲酸乙腈溶液提取,使用PRiME HLB固相萃取柱净化,收集流穿液氮吹至近干,使用0.1%甲酸水∶乙腈(9∶1,v/v)复溶后,使用UPLC-MS/MS正电喷雾电离源,多反应检测(Multiple reaction monitoring,MRM)模式测定结果,并采用基质匹配外标法定量。结果显示,76种药物的检出限为0.3～0.8μg/kg,定量限为0.5～2.0μg/kg;在LOQ、2倍LOQ和5倍LOQ等3个浓度下,76种药物的平均回收率为56.63%～116.86%,批内相对标准偏差为0.50%～18.91%,批间相对标准偏差为0.17%～23.04%。表明建立的方法准确可靠,操作简便,适用于鸡蛋中药物多残留的快速分析检测。 相似文献
4.
笔者建立了超高效液相色谱-串联质谱法(UPLC/MS/MS)检测鸡蛋中金刚烷胺的新方法。采用三氯乙酸溶液和庚烷磺酸钠溶液作为样品的提取溶液,经HLB固相萃取柱净化后上机测定。在正离子模式下通过两对离子对进行定性和定量分析。结果显示,金刚烷胺在1μg/L~50μg/L范围内线性关系良好,相关系数r大于0.9990;空白鸡蛋在2μg/kg、5μg/kg、10μg/kg添加浓度上的回收率均在75%~112%之间;批内及批间相对偏差(RSD)均小于18%;本方法的定量限为2μg/kg(S/N10),检测限为1μg/kg(S/N3)。 相似文献
5.
为建立鸡蛋中氯羟吡啶残留的高效液相色谱法,经乙腈提取净化鸡蛋试样中残留的氯羟吡啶,以磷酸盐缓冲溶液-乙腈(85+15)为流动相,采用C18色谱柱,标准曲线在0.025～2μg/mL浓度内呈线性相关,相关系数(R2)为0.9999;在空白鸡蛋样品中添加0.05mg/kg(定量限)、1mg/kg、2.5mg/kg、5mg/kg的氯羟吡啶,回收率为70%～110%,相对标准偏差(RSD)小于10%。该方法简单快速,灵敏度高,重现性好,适合鸡蛋中氯羟吡啶药物残留的测定。 相似文献
6.
建立超高效液相色谱-串联质谱法(Ultrahigh-performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定鸡蛋中5种磺胺类药物(磺胺甲恶唑、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺喹噁啉、磺胺二甲氧嘧啶)和甲氧苄啶的残留量的方法。样品经乙腈提取2次, 95%乙腈溶液进行溶解后,过Alumina B Cartridges柱,30%乙腈洗脱,滤膜过滤后滤液用于超高效液相色谱-串联质谱仪测定,外标基质标准曲线法定量。在0.5～100μg/kg的浓度范围内5种磺胺类药物和甲氧苄啶色谱峰面积与浓度呈良好线性相关,相关系数均大于0.99;方法检测限0.5μg/kg、定量限为1.0μg/kg;鸡蛋样品中5种磺胺类药物和甲氧苄啶在1.0～100.0μg/kg添加水平内的平均回收率在66.3%～97.5%之间,批内、批间相对标准偏差在1.4%～11.4%之间。该方法回收率满足残留检测要求,且方法的重现性良好,满足国内外兽药残留相关法规规定。 相似文献
7.
建立了一种简单、实用的鸡蛋中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ残留的凝胶渗透色谱-超高效液相色谱检测方法。样品用乙腈∶丙酮=9∶1（V/V）溶液提取,经凝胶渗透色谱（GPC）净化后,反相液相色谱分离测定。本方法的检测限为20μg/kg,定量限为50μg/kg。四种苏丹红染料在20～2000 ng/mL范围内呈线性相关。在空白鸡蛋中添加50～1000μg/kg浓度下,四种苏丹红的平均回收率为65%～85%,批内变异系数在1.0%～4.8%之间（n=5）,批间变异系数在2.1%～5.9%之间（n=3）。结果表明,该法简单、灵敏、特异性强、重现性好,适用于鸡蛋中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ残留的测定。 相似文献
8.
为探索一次性检测猪肉中多种磺胺类药物残留的检测方法,建立了同时测定猪肉中22种磺胺类药物残留的固相萃取-超高效液相色谱方法。样品用3%乙酸乙腈提取,MCX固相萃取柱净化,水和甲醇淋洗,5%氨化甲醇洗脱,氮气吹至近干,0.1%甲酸-乙腈(9:1,V/V)溶液复溶,二极管阵列检测器270 nm检测。结果显示:该方法对22种磺胺类药物检测的线性关系良好(R2 0.999),定量限为2.5～10.0μg/kg,检测限为1.0～4.0μg/kg;各药物平均回收率为83.2%～96.6%,批内和批间变异系数分别为1.1%～3.5%和3.6%～13.4%。结果表明,该方法灵敏度高、重复性好、成本低廉,且操作简单、快速,可用于猪肉样品中多种磺胺类药物残留的同时检测。 相似文献
9.
为了测定牛肌肉、肝脏、肾脏组织中双氯芬酸钠的残留量,研究建立了一种用于该检测的高效液相色谱-串联质谱(LC-MS/MS)方法。试验将样品中加入乙腈提取液重复提取2次,超声波辅助提取,提取液中加入C18、PSA混合吸附剂进行净化。色谱柱采用C18反相柱对药物进行分离,洗脱液采用乙腈-0.1%甲酸水进行等度洗脱,配备电喷雾离子源,药物在正离子模式下电离,多反应监测模式(MRM)分段扫描测定检测结果,并采用内标法定量分析。结果表明,双氯芬酸在0.5～100μg/L浓度范围内有良好的线性关系,相关系数大于0.99;在牛的肌肉、肝脏和肾脏组织中检测限(LOD,S/N=3)为0.5μg/kg,定量限(LOQ,S/N=10)为1.0μg/kg。在3个浓度添加水平下,平均回收率为97.7%～114%,日内变异系数0.5%～4.7%,日间变异系数为0.9%～7.5%。该方法操作简便、结果准确,满足兽药残留检测方法规定要求,运用于快速准确测定牛肌肉、肝脏、肾脏等组织中双氯芬酸钠的残留。 相似文献
10.
《中国家禽》2021,(10)
为了快速高效测定鸡肉和鸡蛋中5种利尿剂(卞氟噻嗪、氯噻嗪、氯噻酮、呋塞米、氢氯噻嗪)的残留量,样品经过乙腈试剂和萃取盐提取,用Bond Elut QuEChER净化柱净化,建立了一种超高液相色谱-串联质谱法(UPLC-MS/MS)方法。结果显示:5种利尿剂在1～200 ng/mL范围内具有良好的线性相关性,相关系数均大于0.99;建立的方法检测限在0.5～1.0μg/kg,定量限在1.5～2.0μg/kg;鸡蛋和鸡肉中5种利尿剂药物在2～200.0μg/kg添加范围内平均回收率在60.8%～108.7%,批内、批间相对标准偏差的范围为0.9%～11.4%。研究表明建立的UPLC-MS/MS方法操作方便、结果准确、高效、重现性好,符合兽药残留标准检测的相关要求,可用于禽产品利尿剂残留的快速检测。 相似文献
11.
Owen J Slocombe D McMillan I 《The Canadian veterinary journal. La revue veterinaire canadienne》1986,27(9):324-328
In late December 1985, 1485 institutional veterinarians and small and mixed animal clinics across Canada were sent a questionnaire in order to assess the status of Dirofilaria immitis in Canada in 1985 and 44% of them responded. Veterinarians reported that 137,300 dogs were blood-tested to check for microfilariae and 1210 dogs were found with heartworm. Another 36 dogs were amicrofilaremic but diagnosed with heartworm disease to give the total number diagnosed in 1985 as 1247 (0.91%).
Heartworm was reported from all provinces except Prince Edward Island, Newfoundland and Saskatchewan but most (1126) of the cases were in Ontario. Southwestern Ontario continued to be the primary focus of the infection in Canada. From Quebec, 91 cases were reported mostly from and around Montreal. From Manitoba, 19 cases were reported from Winnipeg and surrounding areas. Heartworm was found most frequently in companion dogs over three years of age maintained mainly outdoors in rural areas. About 28% of the cases were observed with clinical signs of heartworm disease and 78% had a history of not having left Canada.
相似文献12.
Slocombe JO McMillan I 《The Canadian veterinary journal. La revue veterinaire canadienne》1989,30(6):504-508
In late November 1988, 1581 small and mixed animal clinics and institutional veterinarians across Canada were sent a questionnaire in order to assess the status of Dirofilaria immitis in Canada in 1988, and 46% of them responded. Veterinarians reported that 181,577 dogs were blood-tested for heartworm disease and 367 dogs were found with D. immitis microfilariae. Another 60 dogs were amicrofilaremic but diagnosed with heartworm disease to give the total number of cases diagnosed in 1988 as 441 (0.24%). 相似文献
13.
Slocombe JO McMillan I 《The Canadian veterinary journal. La revue veterinaire canadienne》1985,26(10):323-327
In late December 1984, 1853 institutional veterinarians and small and mixed animal clinics across Canada were sent a questionnaire in order to assess the status of Dirofilaria immitis in Canada in 1984 and 35% of them responded. Veterinarians reported that 97,794 dogs were blood-tested to check for microfilariae and 1417 dogs (1.45% of those tested) were found with heartworm. Another 34 dogs were amicrofilaremic, but were diagnosed as having heartworm disease, to give the total number diagnosed in 1984 as 1451 (1.48%). Heartworm was reported from all provinces except Prince Edward Island and Newfoundland but most (1310) of the cases were in Ontario. In Quebec, 126 cases were reported mostly from west of Montreal.
Heartworm was found most frequently in companion dogs over three years of age maintained mainly outdoors in rural areas. About 27% of the cases were observed with clinical signs of heartworm disease and 72% had a history of not having left Canada. Southwestern Ontario continued to be the primary focus of the infection.
相似文献14.
15.
Slocombe JO Villeneuve A 《The Canadian veterinary journal. La revue veterinaire canadienne》1993,34(10):630-633
In late November 1991, 1883 clinics in Canada were sent a questionnaire to assess the status of Dirofilaria immitis in dogs in 1991 and there was a 60.0% response. There were 344,031 dogs tested for heart-worm (HW), 627 were found infected and the prevalence of HW infection was 0.18%. There were 417 dogs with HW in Ontario, 116 in Manitoba, 38 in Quebec, 53 in British Columbia, three in Alberta, and one in Nova Scotia. In British Columbia, all of the infected dogs but one were from the Okanagan valley which, as from 1991, is a new focus of infection in Canada. Most dogs with HW had not been on preventive medication in 1990, and the prevalence among dogs tested and unprotected was 0.59%. That prevalence was considerably higher in endemic areas. Companion dogs, over three years of age and maintained primarily outdoors in rural areas, were most frequently infected. One cat was diagnosed with D. immitis and 33 dogs had Dipetalonema reconditium. 相似文献
16.
In late November 1989, 1732 clinics and institutional veterinarians were sent a questionnaire to assess the status of Dirofilaria immitis, and 51.7% responded. Of 247,716 dogs tested, 394 had D. immitis microfilariae and 51 were amicrofilaremic for a total of 445 cases and heartworm prevalence of 0.17%. Most (408) of these dogs had no preventive medication and the prevalence among dogs tested and unprotected was 1.01%. That prevalence was considerably higher in endemic areas. Thirty-seven dogs with heartworm had preventive medication. Heartworm was most frequent in companion dogs over three years of age maintained outdoors in rural areas. About 75% of the cases had never left Canada, 26% had clinical signs and 125 were not treated.
Heartworm was reported from British Columbia, Manitoba, Ontario, Quebec, Nova Scotia and Newfoundland, but 383 cases were in Ontario. South-western Ontario was the primary focus of infection. There were 33 cases in Quebec and 24 in Manitoba, mainly found in and around Metropolitan Montreal and Winnipeg respectively.
相似文献17.
Slocombe JO McMillan I 《The Canadian veterinary journal. La revue veterinaire canadienne》1988,29(8):641-646
In late November 1987, 1246 institutional veterinarians and small and mixed animal clinics across Canada were sent a questionnaire in order to assess the status of Dirofilaria immitis in Canada in 1987, and 50% of them responded. Veterinarians reported that 165,428 dogs were blood tested for heartworm disease and 511 dogs were found with D. immitis microfilariae. Another 78 dogs were amicrofilaremic but diagnosed with heartworm disease to give the total number of cases diagnosed in 1987 as 589 (0.35%). 相似文献
18.
Owen J Slocombe D McMillan I 《The Canadian veterinary journal. La revue veterinaire canadienne》1987,28(8):491-495
In late December 1986, 1224 institutional veterinarians and small and mixed animal clinics across Canada were sent a questionnaire in order to assess the status of Dirofilaria immitis in Canada in 1986; 46% of them responded. Veterinarians reported that 150,989 dogs were blood-tested for microfilariae and 869 dogs were found with heartworm. Another 65 dogs were amicrofilaremic but diagnosed with heartworm disease and one was found with heartworm at necropsy to give the total number diagnosed in 1986 as 935 (0.62%).
Heartworm was reported from Manitoba, New Brunswick, Ontario and Quebec, but most (810) of the cases were from Ontario. South-western Ontario continued to be the primary focus of the infection in Canada. There were 103 cases reported from Quebec, mostly from and around Montreal, and 21 cases from Manitoba, from Winnipeg and surrounding areas. Heartworm was found most frequently in companion dogs over three years of age maintained mainly outdoors in rural areas. About 33% of the cases were observed with clinical signs of heartworm disease and 81% had a history of not having left Canada.
相似文献19.
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Slocombe JO McMillan I 《The Canadian veterinary journal. La revue veterinaire canadienne》1984,25(9):347-350
In late December 1983, 2 800 veterinarians across Canada were sent a questionnaire in order to assess the status of heartworm disease in Canada in 1983 and 26% of them responded. Veterinarians reported that 59 504 dogs were blood-tested to check for microfilariae and 771 dogs (1.30% of those tested) were found with Dirofilaria immitis. Heartworm disease was diagnosed in all provinces except New Brunswick and Newfoundland but most (733) of the cases were in Ontario.
Heartworm disease was found most frequently in companion dogs over three years of age maintained mainly outdoors in rural areas. About 31% of the cases were observed with clinical signs of heartworm disease and 64% had a history of not having left Canada. Southwestern Ontario continues to be the focus of the infection and most of the dogs there had not left the province previously.
相似文献