气相色谱串联质谱法检测饲料中的盐酸克伦特罗

盐酸克伦特罗作为一种主要的β-兴奋剂应用于畜禽肉制品生产中,用以提高肌肉和脂肪的比例并加快生长速度。在畜禽产品中过量残留会对消费者造成危害,因此被禁止在畜禽养殖中使用。盐酸克伦特罗在家畜与人体内吸收好,而且与其他β-兴奋相比,它的利用率高,以至食用了含有盐酸克伦特罗的猪肉出现中毒现象。由于盐酸克伦特罗通过饲料对动物的饲喂会残留在动物的肌肉与内脏组织中,对饲料中盐酸克伦特罗进行监测也就显得尤为重要。经试验,应用气相色谱串联质谱法检测饲料中盐酸克伦特罗,标准曲线r≥0.99999;变异系数(CV值)≤0.91%;检测回收率88.2%～98.2%;回收率标准偏差≤1.47%。     

饲料中盐酸克伦特罗的测定-HPLC法

盐酸克伦特罗(CLB)作为一种主要的β-兴奋剂应用于畜禽肉制品生产中,用以提高肌肉和脂肪的比例并加快生长速度.在畜禽产品中过量残留会对消费者造成危害,因此被禁止在畜禽养殖中使用.CLB在家畜与人体内吸收好,而且与其他β-兴奋剂相比,它的利用率高,以至食用了含有盐酸克伦特罗的猪肉出现中毒现象.由于CLB通过饲料对动物的饲喂会残留在动物的肌肉与内脏组织中,对饲料中CLB进行监测也就显得尤为重要.经试验,应用高效液相色谱(HPLC)法检测饲料中盐酸克伦特罗,标准曲线r值≥0.999 95;变异系数(CV值)≤0.82%;检测回收率88.06%～100.33%;回收率标准偏差≤1.25%.     

农业部和国家药品监督管理局以农牧发《2000》4号文“关于查处非法生产、销售和使用盐酸克伦特罗等药品”的紧急通知

近来 ,一些企业和饲养场家为牟取暴利 ,非法生产、销售和使用盐酸克伦特罗等药品 ,严重违反了《中华人民共和国药品管理法》、《饲料和饲料添加剂管理条例》及《药品流通监督管理办法》。为了加强对药品生产和流通的管理 ,杜绝在饲料和饲料添加剂以及饲养过程中非法使用盐酸克伦特罗等药品 ,农业部和国家药品监督管理局决定在全国范围内对非法生产、销售和使用盐酸克伦特罗等药品的行为进行查处。现将有关事宜通知如下 :１各省（自治区、直辖市）畜牧兽医、饲料和药品监督管理部门要迅速组建查处非法生产、销售和使用盐酸克伦特罗等药品联合…     

动物组织和尿液中盐酸克伦特罗的快速检测

<正> 盐酸克伦特罗(Clenbuterol),俗称“瘦肉精”,是一种β-兴奋剂。农业部已发布通告,禁止在饲料中使用,动物组织和尿液中不得检出。但仍有一些不法饲料生产商及养殖业主在饲料中掺入,用以提高瘦肉率和促进动物生长。盐酸克伦特罗通过饲料残留在动物组织中,人摄入残留在食品中的盐酸克伦特罗,会产生心跳过快、心慌、不自主颤抖、双脚站不住、心悸胸闷、四肢肌肉颤动、头晕乏力等神经中毒后失控的现象,甚至死亡,尤其对高血压、心脏病、糖     

气相色谱-串联质谱法测定饲料中的瘦肉精

盐酸克伦特罗也称为"瘦肉精",可作为一种主要的β-兴奋剂应用于畜禽肉制品生产中,用以提高肌肉和脂肪的比例并加快生长速度。在畜禽产品中过量残留会对消费者造成危害,因此在畜禽养殖中被禁止使用。盐酸克伦特罗在家畜与人体内易吸收,而且与其它β-兴奋剂相比,它的利用率更高,以致食用了含有盐酸克伦特罗的猪肉出现中毒现象。由于盐酸克伦特罗会残留在动物的肌肉与内脏组织中,对饲料中盐酸克伦特罗进行监测也就显得尤为重要。经试验,应用GC-MS法检测饲料中盐酸克伦特罗,标准曲线r值≥0.99999;变异系数(CV值)≤0.91%;检测回收率:88.2%～98.2%;回收率标准偏差≤1.47%。     

应用气质联用法检测饲料中盐酸克伦特罗的探讨

盐酸克伦特罗作为一种主要的β-兴奋剂应用于畜禽肉制品生产中,用以提高肌肉和脂肪的比例并加快生长速度。在畜禽产品中过量残留会对消费者造成危害,因此被禁止在畜禽养殖中使用。盐酸克伦特罗在家畜与人体内吸收好,而且与其他β-兴奋剂相比,它的利用率高,以致于食用了含有盐酸克伦特罗的猪肉出现中毒现象。由于盐酸克伦特罗易残留在动物的肌肉与内脏组织中,对饲料中盐酸克伦特罗进行监测显得尤为重要。经试验,应用GC-MS法检测饲料中盐酸克伦特罗,标准曲线r值≥0.99999;变异系数(CV值)≤0.91%;检测回收率:88.2%~98.2%;回收率标准偏差≤1.47%。     

中华人民共和国农业部公告

国家明令禁止在饲料和动物饮用水中添加盐酸克伦特罗等药品。广东中洋饲料有限公司置国家法律法规于不顾，非法生产、经营含有盐酸克伦特罗的添加剂预混合饲料，造成广东省河源市４８４名居民中毒，情节特别严重，社会影响极坏。根据《饲料和饲料添加剂管理条例》第三十条规定，现吊销其添加剂预混合饲料生产许可证，取消其从业资格。 特此公告中华人民共和国农业部公告$中华人民共和国农业部     

对盐酸克伦特罗的再认识及其检测方法

应用盐酸克伦特罗作饲料添加剂来提高瘦肉率和减少脂肪沉积，曾经是一种有效的方法，但近年来研究证明它对动物和人体有残留危害。欧美已禁用此药，我国政府也明令禁止生产、销售、使用盐酸克伦特罗药物，但仍有少数生产厂家在进行违法操作。本文就盐酸克伦特罗的使用历程、残留危害、检测方法及我国目前的禁用情况进行阐述，以便饲料生产者提高认识，从而支持、拥护、贯彻执行我国政府的禁令。     

^14C—盐酸克伦特罗混饲在猪体内的残留消除研究

克伦特罗是一种β-兴奋剂,添加于饲料中能提高几种家畜包括猪的瘦肉率.由于其在黑市可买到,克伦特罗在欧洲、美国、亚洲非法用于家畜.在某些国家,非法用过克伦特罗的牛组织中的残留引起人的中毒.最近有人报道,人食用了含有克伦特罗的猪肉导致中毒.     

关于查处非法生产、销售和使用盐酸克伦特罗等药品的紧急通知

农业部4月3日,向各省、自治区、直辖市(农牧、农业)厅(局)、饲料工业办公室、卫生厅(局)、药品监督管理部门下发了“关于查处非法生产、销售和使用盐酸克伦特罗等药品的紧急通知”,通知指出: 近来,一些企业和饲养场家为牟取暴利,非法生产、销售和使用盐酸克伦特罗等药品,严重违反了《中华人民共和国药品管理法》、《饲料和饲料添加剂管理条例》及《药品流通监督管理办法》。为了加强对药品生产和流通的管理,杜绝在饲料和饲料添加剂以及饲养过程中非法使用盐酸克伦特罗等药品,农业部和国家药品监督管理局决定在全国范围内对非法生产、销售和使用盐酸克伦特罗等药品的行为进行查处。现将有关事     

应用GC-MS测定动物组织及尿中克仑特罗残留

对酶联免疫法筛选检出的阳性猪肝和猪尿样品应用GC-MS法进行了确证试验,分析了操作中衍生化、质谱参数的设定、溶剂的干扰、进样及谱库的检索等因素对测定结果的影响,说明了应注意的问题并提出了解决问题的方法,可供残留分析工作者参考.     

猪屠宰检疫方法与处理措施

我国畜牧养殖产业迅猛向前发展,养殖规模扩大的同时,各种养殖安全问题凸显,瘦肉精、毒奶粉等事件频繁爆发,使食品安全问题备受社会大众关注。猪肉作为人们日常餐桌上的蛋白质来源,品质和质量会对消费者的身心健康产生严重威胁。为更好地贯彻动物防疫法规和生猪屠宰检疫管理条例,确保消费者吃上放心肉,需要严格按照国家相关规定要求开展生猪屠宰检疫,并按照程序对确诊带病的猪肉制品进行严格的无害化处置,避免带病动物上市销售威胁消费者身心健康。该文论述猪屠宰检疫方法和带病猪肉组织的处置措施。     

从部分兽药残留检测状况浅谈畜产品质量安全

阐述了青霉素、喹乙醇、盐酸克仑特罗、阿苯达唑、磺胺类等部分兽药残留对人体的危害及残留检测现状,表明畜产品质量安全存在隐患;分析了造成兽药残留的各种原因,并就如何控制兽药残留提高畜产品质量提出对策.     

用HPLC-MS/MS研究动物毛发中克伦特罗的残留及代谢规律

研究建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定毛发中盐酸克伦特罗残留的方法。猪毛发以0.1moL/L盐酸溶液提取,MCX固相萃取柱净化,流动相溶解定容。以SB-C18柱为分离柱,1%乙酸水溶液和甲醇(60∶40,V∶V)作为流动相,MS/MS进行定性和定量分析。在优化条件下的最低检出限为0.05μg/kg,定量限为0.2μg/kg。毛发样品中添加不同浓度盐酸克伦特罗,测得回收率在79.0%～86.2%之间,变异系数均低于15.2%。应用该方法研究了盐酸克伦特罗在猪毛发中的代谢并初步探讨其代谢机理。结果表明:在较高饲喂浓度(10mg/kg)时,用药5d后,黑色猪毛发有少量盐酸克伦特罗残留,而白色猪毛发中未检出。从第7天起猪毛发中盐酸克伦特罗蓄积量逐渐增加,最高蓄积浓度为4852.5μg/kg。     

克伦特罗在猪体内立体选择性降解行为研究

为了解克伦特罗在猪体内是否存在立体选择性降解行为,手性分离制备了克伦特罗单一对映体,然后对生猪进行饲喂含有克伦特罗外消旋体(2.0 mg/kg)和单一对映体(1.0 mg/kg)的饲料,7 d后进行屠宰,定期采集猪的肌肉、肝脏、肾脏、心脏、肺脏和尿液,测定克伦特罗对映体含量。结果表明,克伦特罗在猪体内存在立体选择性降解行为,肝脏、肾脏和肺脏中对映体(右旋体/左旋体)比例较高,心脏和肌肉中的对映体比例相对较低;休药3 d时,肝脏、肾脏、猪尿中的对映体比例均处于最高点。同时克伦特罗对映体在猪体内不存在相互转化现象。该研究为科学评估动物性食品残存的克伦特罗对人体健康造成的危害提供了科学依据。     

Clenbuterol hydrochloride in calves with a natural bovine respiratory syncytial virus infection

The effect of clenbuterol hydrochloride on the course of disease in calves with a natural bovine respiratory syncytial virus infection was examined. Six calves (three to nine months of age) originating from four herds with respiratory tract disease and serological evidence of a bovine respiratory syncytial virus infection were used in this study. The calves were injected intravenously with clenbuterol hydrochloride. The effect of clenbuterol on the course of disease was measured using the PO2 in blood taken from an indwelling canula inserted in the caudal auricular artery and by clinical signs. Clenbuterol did not improve clinical signs. After clenbuterol administration arterial PO2 values decreased significantly in five out of six patients. Six to eight hours after medication the mean arterial PO2 values were higher than initial values. The moderate positive effect of clenbuterol after six to eight hours may be caused by enhancing ciliary activity and by the secretolytic activity of clenbuterol.     

GC/MS法研究猪体内盐酸克伦特罗的残留代谢规律

样品用乙酸乙酯提取,盐酸溶液萃取后,再经SCX固相萃取柱净化,50℃水浴中氮气吹干后衍生化。以气相色谱-质谱选择86、212、262、277四个碎片离子进行定性定量分析。盐酸克伦特罗在0.01～2.0 mg/L成线性（R2为0.999）,猪肉中3种不同添加浓度0.01、0.10和0.20mg/kg下克仑特罗平均回收率分别为88.31%、92.85%、93.97%,相对标准偏差分别为5.26%、7.58%、4.59%,样品中最低检测限（S/N=3）为0.1 ug/kg。应用该方法研究了克仑特罗在猪体内的消除并初步探讨其代谢机理。结果表明,在饲喂浓度（3 mg/kg）1个月后,猪体内盐酸克伦特罗蓄积量不算太高,最高蓄积浓度为493.59 ug/kg,而且停药后代谢又非常快。     

Total radioactive residues and clenbuterol residues in swine after dietary administration of [14C]clenbuterol for seven days and preslaughter withdrawal periods of zero, three, or seven days

Nine barrows (23.8 +/- 0.9 kg) and 9 gilts (23.1 +/- 0.9 kg) were used to determine the disposition of radiocarbon after oral [14C]clenbuterol (4-amino-alpha-[t-butylaminomethyl]-3,5-dichlorobenzyl [7-(14)C]alcohol hydrochloride) administration and to determine total and parent residues in edible tissues. Three barrows and three gilts, housed in metabolism crates, were fed 1 ppm [14C]clenbuterol HCl for seven consecutive days in three separate trials; a single barrow and gilt from each trial was slaughtered after 0-, 3-, or 7-d preslaughter withdrawal periods. Urine and feces were collected during the dosing and the withdrawal period; edible and inedible tissues were collected at slaughter. Total recovery of radiocarbon was 94.2 +/- 6.5%. Total clenbuterol absorption was greater than 75% for barrows and 60% for gilts. Total radioactive residues in tissues were not different (P > 0.05) between barrows and gilts. Concentrations of parent clenbuterol in liver, kidney, skeletal muscle, adipose tissue, and lung did not differ between barrows and gilts (P > 0.05). Total radioactive and parent residues declined in tissues as withdrawal period increased. After the 0-d withdrawal period, total liver residues (286 ppb) were approximately equal to lung residues, twice those of the kidney, and about 15 times those of adipose tissue and skeletal muscle. After a 7-d withdrawal period, total radioactive residues in liver (15 ppb) were roughly three times greater than lung, kidney, and adipose tissue total residues and about 13 times those of skeletal muscle total residues. Parent clenbuterol represented 79, 63, 42, 67, and 100% of the total radioactive residue in adipose tissue, kidney, liver, lung, and skeletal muscle, respectively, in hogs slaughtered with a 0-d withdrawal period. With increasing withdrawal period, the percentage of total radioactive residue present as parent clenbuterol within edible tissues (including lung) decreased, so that after a 7-d withdrawal period, 7, 16, and 29% of the total residue was composed of parent clenbuterol in kidney, liver, and lung, respectively. After a 7-d withdrawal period, parent clenbuterol exceeded the European maximum residue limit (0.5 ppb) 4.6-fold in liver and 2.4-fold in lung. In muscle, clenbuterol was approximately 40 times the limit after a 0-d withdrawal period but had dropped below 0.5 ppb after a 3-d withdrawal period. Results from this study indicate that clenbuterol HCl is well absorbed in swine and that the use of clenbuterol in this species in an off-label manner is inconsistent with human food safety standards used in developed countries.     

中国与美国、欧盟、日本和CAC猪组织中兽药残留限量标准的对比研究

为便于中国兽药残留标准的改进和相关法规体系的建立提供参考,同时为中国畜产品贸易提供数据参考,保障人们的饮食安全,促进中国畜产品经济的更好发展,本研究首先对中国新国标GB 31650-2019《食品安全国家标准食品中兽药最大残留限量》中规定的猪组织中兽药残留种类和兽药最大残留限量（MRLs）标准进行了简单分析;然后对美国、欧盟、日本和食品法典委员会（CAC）规定的猪组织中兽药残留种类和兽药MRLs标准与中国新国标进行对比,通过对规定兽药总数、中国没有规定而其他标准有规定的兽药种类、其他标准严于中国标准的兽药种类等几项内容的比较,找出差异。结果显示,中国新国标做出了更加详细的补充和修改;从整体上来看,中国规定的猪组织中兽药MRLs标准越来越完善,大部分标准与欧盟、美国、日本和CAC规定标准的差距也越来越小,然而在部分种类兽药MRLs标准的规定方面和这些国家或组织仍有一定的差距。中国需加强与各个发达国家和组织的交流与合作,推进中国的兽药残留标准的发展,加快对动物产品质量安全标准的更新。     

Distribution and elimination of clenbuterol in tissues and fluids of calves following prolonged oral administration at a growth-promoting dose

A pharmacokinetic study is described in which Friesian calves (n = 30) were treated orally with clenbuterol at 10 times the therapeutic dose. The study was designed to establish the distribution and elimination of clenbuterol from edible tissues, the major compartments of the eye and body fluids. Animals (n= 24) were dosed (10 μg/kg body weight) twice daily with clenbuterol for 21 days and slaughtered in groups of five (one untreated control animal per group) at 6 h and 1, 2, 4, 8 and 16 days after cessation of treatment At slaughter, samples of diaphragm muscle, liver, kidney, bile, urine and both eyes were obtained. One of the eyes was separated into constituent tissues: aqueous humour, vitreous humour, comea, lens, retina (without pigmented epithelium), choroid (with pigmented retinal epithelium; choroid/PRE) and sclera. All samples were stored at -20°C. Clenbuterol concentrations were higher in liver than kidney, bile and urine from day 2 of withdrawal onwards. Concentrations in choroid/PRE were at least 10 times higher than in liver at all periods following cessation of treatment and 52 times higher 16 days after treatment The concentrations of clenbuterol in the constituent tissues of the eye were in the order choroid/PRE > comea > sclera > retina > aqueous humour/vitreous humour ≥ lens. Concentrations of clenbuterol in choroid/PRE taken from eyes frozen whole were generally lower than those in choroid/PRE separated before storage. Choroid/PRE stored by either method contained clenbuterol at more than 100 ng/g 16 days following cessation of treatment These data suggest that analysis of choroid taken at the abattoir would provide reliable surveillance information on the use or abuse of clenbuterol within the slaughter population. It is proposed that liver samples taken concurrently could be used in the event of a positive result from choroid/PRE analysis to indicate whether the maximum residue limit for edible tissues has been exceeded.