黄鳝肌肉中的20种性激素同时测定的气质联用检测方法

食品科学 ›› 2008, Vol. 29 ›› Issue (6): 298-303.

黄鳝肌肉中的20种性激素同时测定的气质联用检测方法

湛嘉, 俞雪钧, 李佐卿, 谢东华, 樊苑牧, 陈树兵

宁波出入境检验检疫局；宁波出入境检验检疫局浙江宁波315012；浙江宁波315012；

出版日期:2008-06-15 发布日期:2011-08-26

Stimultaneous Determination of Residue of Sex Hormones in Eel Muscle by Gas Chromatography-Mass Spectrometry

ZHAN Jia, YU Xue-Jun, LI Zuo-Qing, XIE Dong-Hua, FAN Yuan-Mu, CHEN Shu-Bing

Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China

Online:2008-06-15 Published:2011-08-26

摘要/Abstract

摘要： 建立了用安捷论GC-MS5975对黄鳝肌肉中20种性激素能同时进行筛选、定量和确证的灵敏、特异可靠的检测方法。对5.0g肌肉样品,采用β-葡糖苷酸酶(来自Helix pomatia)对提取物水解后,经叔丁基甲醚提取,异辛烷脱脂,经脱脂棉过滤后进入C18小柱,再经NH2小柱净化后七氟丁酸酐对其进行衍生,最后利用GC-MS进行检测。采用外标法定量,通过对空白样品添加标准品,使之理论含量为1、2.5和5μg/kg,追宝龙按相应水平的5倍添加,以S/N≥3,甲睾酮、去氢睾酮和甲孕酮,检出限为0.25μg/kg,除了追宝龙的检测限为5μg/kg外,其他的检出限均为0.5～1μg/kg。对待测物三个水平的添加回收实验表明,平均回收率范围为79.8%～106.3%,平均变异系数的范围为11.6%～17.9%。当添加水平为1μg/kg(追宝龙为结果5μg/kg),本方法不同批次回收率的相对偏差范围为9.3%～22.1%,重复性好。因此,本方法对目前动物源食品中的性激素监督检验有参考价值。

关键词: 性激素, 气相色谱-质谱联用, 黄鳝

Abstract: A highly sensitive, specific and credible method for the simultaneous determination of 20 sex hormones in muscle of swamp eel performed by GC-MS(Agilent 5975) was studied.Muscle tissues of swamp eel (5.0 g) were hydrolyzed by glucuronidase from Helix pomatia juice, extracted by tert-butyl methyl ether, defatted by iso-octane, and cleaned-up through dual columns of C18 and NH2. The extracts obtained were derivatized with heptafluorobutyric anhydride, following formation of the di-heptafluorobutyryl (di-HFB) derivative, and then identification and quantification were carried out by means of capillary gas chromatography-mass spectrometry. For quantitation, the external standards were used and the method was validated with blank samples fortified at 1, 2.5 and 5 μg/kg with 5.0 g sample(trenbolone spiked 5 times as others). Results showed that the detection limits are 0.25～5μg/kg for all analytes. Average recovery (%) and coefficient of variance range from79.8% to 106.3%, and from 11.6% to 17.9%, respectively. The relative standard deviation (RSD) ranges from 9.3% to 22.1% at 1 mg/kg spiked level. The study results showed that the recovery and repeatability are good. Therefore, the method is very useful for the animal food quality surveillance at present.

Key words: sex hormone, GC-MS, swamp eel

湛嘉, 俞雪钧, 李佐卿, 谢东华, 樊苑牧, 陈树兵. 黄鳝肌肉中的20种性激素同时测定的气质联用检测方法[J]. 食品科学, 2008, 29(6): 298-303.

ZHAN Jia, YU Xue-Jun, LI Zuo-Qing, XIE Dong-Hua, FAN Yuan-Mu, CHEN Shu-Bing. Stimultaneous Determination of Residue of Sex Hormones in Eel Muscle by Gas Chromatography-Mass Spectrometry[J]. FOOD SCIENCE, 2008, 29(6): 298-303.

[1]	刘玉兰，舒垚，孙国昊，马宇翔，姜元荣，陈宁. 花生品种对花生酱风味及综合品质的影响[J]. 食品科学, 2021, 42(9): 15-21.
[2]	刘盼盼，郑鹏程，龚自明，常泽睿，苏方俊，黄波，冯琳，高士伟，郑琳. 橘红茶香气特征及风味成分分析[J]. 食品科学, 2021, 42(8): 198-205.
[3]	单启梅，赵晓策，罗瑞明，尤丽琴. 滩羊肌肉在煮制过程中可挥发性化合物的变化[J]. 食品科学, 2021, 42(8): 165-171.
[4]	张舒，王长远，冯玉超，盛亚男，富天昕，张艺玮，姜颖俊，于淼，张丽媛. 气相色谱-质谱联用代谢组学技术分析不同产地稻米代谢物[J]. 食品科学, 2021, 42(8): 206-213.
[5]	陈丽花，任丽霞，李东娜，马霞. 甜酒曲中优质酵母菌的分离鉴定及其产香特性分析[J]. 食品科学, 2021, 42(6): 142-149.
[6]	张琴，周丹丹，彭菁，潘磊庆，屠康. 油桃采后结合态香气变化规律及其与可溶性糖的关联性[J]. 食品科学, 2021, 42(6): 206-214.
[7]	程超，夏兰欣，杜芬妮，李伟，田成. 基于9 种风味物质的利川红SPME优化及PLS-DA风味识别[J]. 食品科学, 2021, 42(6): 215-222.
[8]	丁丹，王松磊，罗瑞明，王永瑞，柏霜，沈菲，柏鹤. 基于SPME-GC-MS分析不同烤制时间新疆烤羊腿表层及内层挥发性化合物[J]. 食品科学, 2021, 42(2): 227-234.
[9]	李昊泽，石丽丽，曹学丽，韩天，裴海闰. 风味发酵乳中香精关注成分的筛选及暴露风险评估[J]. 食品科学, 2021, 42(18): 254-260.
[10]	王贺，赵玉红，杨凯. HS-SPME-GC-MS结合电子鼻对10 个品系红松籽油挥发性物质分析比较[J]. 食品科学, 2021, 42(18): 178-184.
[11]	唐莹，贾仕杰，蒋莹，何红英，董丹，王金玲，张健. 红树莓叶茶的制备及与红树莓叶片、绿茶品质的比较[J]. 食品科学, 2021, 42(17): 34-42.
[12]	陈臣，刘政，黄轲，于海燕，田怀香. 基于GC-MS、GC-O及电子鼻评价不同加工方式对乳扇风味的影响[J]. 食品科学, 2021, 42(16): 108-117.
[13]	汤酿，刘静宜，陈小爱，杨玉洁，陈树喜，张子明，周爱梅. 基于GC-MS和GC-IMS联用法分析不同采收期广佛手精油挥发性成分[J]. 食品科学, 2021, 42(16): 193-202.
[14]	符成刚，刘文玉，陈友志，李玉梅，李欢康，周靖，张孔雀，魏长庆. 加热温度对新疆马脂理化性质、脂肪酸及挥发性风味化合物的影响[J]. 食品科学, 2021, 42(16): 54-60.
[15]	王婵，李荣，吴杨，王颖，汤书华，谭津，姜子涛. 调味香料荜茇精油中清除游离基活性成分的快速筛选[J]. 食品科学, 2021, 42(14): 226-231.