利用电感耦合等离子体质谱(ICP-MS)测定中华绒螯蟹中重金属镉的残留量
|
摘要
为建立一种简单、高效检测中华绒螯蟹中重金属镉残留量方法,采用湿法消解及微波消解2种前处理方法,利用ICP-MS测定性腺(G)、肌肉(M)及其两者混合的全部可食部分(B)中的重金属镉残留量,并依据回收率对方法的可靠性进行检验和优化。实验结果表明,在利用湿法消解进行前处理时,G、M、B中镉的检出限范围是0.0025～0.0045μg/g,回收率分别为96.24%±2.13%、99.93%±3.50%和94.74%±1.42%,M的回收率显著高于G和B(P<0.05);同样地,在利用微波消解进行前处理时,G、M、B中镉的检出限范围是0.0012～0.0027μg/g,回收率分别为104.76%±7.40%、92.38%±10.26%和91.850%±4.25%,G的回收率显著高于M和B(P<0.05)。前处理方式影响基质的回收率,不同的前处理适用于处理不同的基质,在处理蟹肉时,最好选择湿法消解法;在处理性腺时,最好选择微波消解法;而处理整个可食部位时,两者都可以。考虑到回收率都能接受,而微波消解法具有用时短、操作简单快速、试剂消耗小等特点,在实际操作时应选择微波消解法进行前处理。
The paper aims to establish a simple and effective detection method for heavy metal cadmium residues in Eriocheir sinensis by using wet and microwave digestion methods.The two pre-treatment methods were tested,using ICP-MS determination of cadmium within the gonads(G),muscles(M)and all edible parts of the animal(B),and their recovery rates were used to compare each method’s reliability.Experimental results from the wet digestion method showed that,for pre-treatment,the detection limit of cadmium in G,M and B was between 0.0025-0.0045μg/g,the recycling rate was 96.24%±2.13%,99.93%±3.50%and 94.74%±1.42%, respectively, and the recovery rate of M was significantly higher than that of G and B(P<0.05).Results from the microwave digestion method revealed that,for pre-treatment,the detection limit of cadmium in G,M and B was between 0.0012-0.0027μg/g,the recycling rate was 104.76%±7.40%,92.38%±10.26%and91.850%±4.25%,respectively,the recovery rate of gonad samples(G)was significantly higher than that of M and B(P<0.05).That the pre-treatment method affected the recovery rate of matrix,and the different pretreatment methods were applicable to different substrates.In handling crab muscle,the best choice was the wet digestion method;while the microwave digestion method was better for gonadal studies.When dealing with the entire edible part,both methods could be reliable.Considering that the recovery rates were acceptable,the microwave digestion method had characteristics of simple,rapid and short operation time,plus less reagent consumption.Therefore,the microwave digestion method should be selected as the pre-treatment method in practical operation.
The paper aims to establish a simple and effective detection method for heavy metal cadmium residues in Eriocheir sinensis by using wet and microwave digestion methods.The two pre-treatment methods were tested,using ICP-MS determination of cadmium within the gonads(G),muscles(M)and all edible parts of the animal(B),and their recovery rates were used to compare each method’s reliability.Experimental results from the wet digestion method showed that,for pre-treatment,the detection limit of cadmium in G,M and B was between 0.0025-0.0045μg/g,the recycling rate was 96.24%±2.13%,99.93%±3.50%and 94.74%±1.42%, respectively, and the recovery rate of M was significantly higher than that of G and B(P<0.05).Results from the microwave digestion method revealed that,for pre-treatment,the detection limit of cadmium in G,M and B was between 0.0012-0.0027μg/g,the recycling rate was 104.76%±7.40%,92.38%±10.26%and91.850%±4.25%,respectively,the recovery rate of gonad samples(G)was significantly higher than that of M and B(P<0.05).That the pre-treatment method affected the recovery rate of matrix,and the different pretreatment methods were applicable to different substrates.In handling crab muscle,the best choice was the wet digestion method;while the microwave digestion method was better for gonadal studies.When dealing with the entire edible part,both methods could be reliable.Considering that the recovery rates were acceptable,the microwave digestion method had characteristics of simple,rapid and short operation time,plus less reagent consumption.Therefore,the microwave digestion method should be selected as the pre-treatment method in practical operation.
引文
[1]张雪娇,苗翠,曹忠军.畜产品中重金属残留的危害及对策[J].畜牧兽医科技信息,2013(6):18-19.
[2]马君贤.重金属镉的环境污染化学[J].当代化工,2007(2):192-194.
[3]皇甫加清.镉对南方鲇抗氧化酶系统和脂质过氧化作用的影响[D].重庆:西南大学,2011.
[4] Alfvdn T, Elinder C, Carlsson M, et al. Low-level cadmium and osteoporosis[J]. J Bone Miner Res,2000,15(8):1579-1586.
[5] Nordberg G. Cadmium and human health:a perspective based on recent studies in China[J]. Trace Elem Exp Med,2003,16(4):307-319.
[6]邓新,温璐璐,迟鑫姝,等.镉对人体健康危害及防治研究进展[J].中国医疗前沿,2010,5(10):4-5.
[7]姚清华,颜孙安,林虬,等.水产品重金属富集规律与风险评估[J].福建农业学报,2014,29(5):498-504.
[8]中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.GB 2762—2017食品安全国家标准食品中污染物限量[S].2017.
[9]陈海槟.水产品中镉、铅、砷的检测方法与应用研究[J].食品安全导刊,2015(15):147-149.
[10]尤炬炬,刘琴,鲍静姣,等.浙江省自然海区梭子蟹重金属残留现状分析[J].现代农业科技,2017(21):190,203.
[11]何佳璐,方力,余新威.舟山市海产品铅、镉、甲基汞污染调查[J].预防医学,2017,29(3):240-242.
[12]李洁傲,赵月然,李军,等.电感耦合等离子体质谱法测定海参中17种金属元素的含量[J].理化检验:化学分册,2016,52(9):1108-1111.
[13]郭雨时,焦阳,娄丽.ICP-MS同时测定水产品中的铅、镉、汞和砷[J].光谱实验室,2012,29(6):3717-3720.
[14]解楠,曹程明,徐红斌,等.微波消解-电感耦合等离子体质谱测定水产品中铅、砷、镉、铬、镍含量[J].食品工业科技,2011,32(7):426-428.
[15]曾海英,王家磊,沈萍萍,等.微波消解-ICP-MS法测定食品、水产品及动物组织中33种金属元素[J].食品安全质量检测学报,2015,6(3):953-961
[16]梁淑轩,王欣,吴虹,等.微波消解/ICP-MS测定水系沉积物中的9种重金属元素[J].光谱学与光谱分析,2012,32(3):809-812.
[17]温中海,苏荣,冼萍.微波消解-ICP/MS法测定水系沉积物中多种元素[J].环境监测管理与技术,2016,28(4):39-42.
[18]方芳,季雨珊,李想,等.ICP-MS研究太湖过滤水和表层沉积物中重金属的含量水平及污染评价[J].光谱学与光谱析,2018,38(4):1245-1250.
[19]蒋天成,刘守廷,罗平,等.微波样品消解-电感耦合等离子体质谱法测定北部湾海产品中重金属的含量[J].理化检验(化学分册),2014,50(1):93-96.
[20]李艳丽,王庚,米浦春,等.3种消解方法在ICP-MS测定沉积物中4种重金属元素的应用[J].光谱实验室,2013,30(2):698-701.
[21]长江流域水环境监测中心.SL219—2013水环境监测规范[M].北京:中国水利水电出版社,1998.
[22]林少美,郑三燕,李瑞芬,等.微波消解-电感耦合等离子体质谱法测定梭子蟹中的10种元素[J].中国卫生检验杂志,2015,25(12):1919-1921.
[23]谭秀慧,朱晓华,杨洪生,等.电感耦合等离子体质谱法测定水产品中铬、铜、锌、砷、镉、铅的含量[J].理化检验(化学分册),2018,54(1):82-85.
[24]李万杰,马春,张新欣,等.微波消解-石墨炉原子吸收法检测海产品中痕量重金属[J].大连工业大学学报,2015,34(2):111-113.
[25]傅春玲,丁薇薇,吴琳,等.微波消解-冷原子荧光光谱法测定中华绒螯蟹中汞的含量[J].国外医学(医学地理分册),2011,32(2):140-142.
[26] Yu Hui-zi, Chen Shun-sheng. Comparison of Volatile Flavor Componentsin Cooked Chinese Mitten Crab Meat and Crab Spawn[J].Food Science,2011,32(08):267-271.
[27]石婧,王帅,龚骏,等.不同育肥方式对中华绒螯蟹雄蟹肌肉呈味物质的影响[J].食品工业科技,2015,36(15):347-351.
[28]刘天天,梁中永,范思华,等.北海沙蟹特征滋味成分的分析[J].食品科学,2018,39(14):236-241.
[29] De Weichen, Min Zhang, Sundar Shrestha Compositional characteristics and nutritional quality of Chinese mitten crab(Eriocheir sinensis)[J].Food Chemistry,2007,103(4):1343-1349
[30]高先楚,王锡昌,顾赛麒,等.中华绒螯蟹性腺加热熟制前后挥发性成分和脂肪酸组成分析[J].现代食品科技,2014,30(9):265-274.
[2]马君贤.重金属镉的环境污染化学[J].当代化工,2007(2):192-194.
[3]皇甫加清.镉对南方鲇抗氧化酶系统和脂质过氧化作用的影响[D].重庆:西南大学,2011.
[4] Alfvdn T, Elinder C, Carlsson M, et al. Low-level cadmium and osteoporosis[J]. J Bone Miner Res,2000,15(8):1579-1586.
[5] Nordberg G. Cadmium and human health:a perspective based on recent studies in China[J]. Trace Elem Exp Med,2003,16(4):307-319.
[6]邓新,温璐璐,迟鑫姝,等.镉对人体健康危害及防治研究进展[J].中国医疗前沿,2010,5(10):4-5.
[7]姚清华,颜孙安,林虬,等.水产品重金属富集规律与风险评估[J].福建农业学报,2014,29(5):498-504.
[8]中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.GB 2762—2017食品安全国家标准食品中污染物限量[S].2017.
[9]陈海槟.水产品中镉、铅、砷的检测方法与应用研究[J].食品安全导刊,2015(15):147-149.
[10]尤炬炬,刘琴,鲍静姣,等.浙江省自然海区梭子蟹重金属残留现状分析[J].现代农业科技,2017(21):190,203.
[11]何佳璐,方力,余新威.舟山市海产品铅、镉、甲基汞污染调查[J].预防医学,2017,29(3):240-242.
[12]李洁傲,赵月然,李军,等.电感耦合等离子体质谱法测定海参中17种金属元素的含量[J].理化检验:化学分册,2016,52(9):1108-1111.
[13]郭雨时,焦阳,娄丽.ICP-MS同时测定水产品中的铅、镉、汞和砷[J].光谱实验室,2012,29(6):3717-3720.
[14]解楠,曹程明,徐红斌,等.微波消解-电感耦合等离子体质谱测定水产品中铅、砷、镉、铬、镍含量[J].食品工业科技,2011,32(7):426-428.
[15]曾海英,王家磊,沈萍萍,等.微波消解-ICP-MS法测定食品、水产品及动物组织中33种金属元素[J].食品安全质量检测学报,2015,6(3):953-961
[16]梁淑轩,王欣,吴虹,等.微波消解/ICP-MS测定水系沉积物中的9种重金属元素[J].光谱学与光谱分析,2012,32(3):809-812.
[17]温中海,苏荣,冼萍.微波消解-ICP/MS法测定水系沉积物中多种元素[J].环境监测管理与技术,2016,28(4):39-42.
[18]方芳,季雨珊,李想,等.ICP-MS研究太湖过滤水和表层沉积物中重金属的含量水平及污染评价[J].光谱学与光谱析,2018,38(4):1245-1250.
[19]蒋天成,刘守廷,罗平,等.微波样品消解-电感耦合等离子体质谱法测定北部湾海产品中重金属的含量[J].理化检验(化学分册),2014,50(1):93-96.
[20]李艳丽,王庚,米浦春,等.3种消解方法在ICP-MS测定沉积物中4种重金属元素的应用[J].光谱实验室,2013,30(2):698-701.
[21]长江流域水环境监测中心.SL219—2013水环境监测规范[M].北京:中国水利水电出版社,1998.
[22]林少美,郑三燕,李瑞芬,等.微波消解-电感耦合等离子体质谱法测定梭子蟹中的10种元素[J].中国卫生检验杂志,2015,25(12):1919-1921.
[23]谭秀慧,朱晓华,杨洪生,等.电感耦合等离子体质谱法测定水产品中铬、铜、锌、砷、镉、铅的含量[J].理化检验(化学分册),2018,54(1):82-85.
[24]李万杰,马春,张新欣,等.微波消解-石墨炉原子吸收法检测海产品中痕量重金属[J].大连工业大学学报,2015,34(2):111-113.
[25]傅春玲,丁薇薇,吴琳,等.微波消解-冷原子荧光光谱法测定中华绒螯蟹中汞的含量[J].国外医学(医学地理分册),2011,32(2):140-142.
[26] Yu Hui-zi, Chen Shun-sheng. Comparison of Volatile Flavor Componentsin Cooked Chinese Mitten Crab Meat and Crab Spawn[J].Food Science,2011,32(08):267-271.
[27]石婧,王帅,龚骏,等.不同育肥方式对中华绒螯蟹雄蟹肌肉呈味物质的影响[J].食品工业科技,2015,36(15):347-351.
[28]刘天天,梁中永,范思华,等.北海沙蟹特征滋味成分的分析[J].食品科学,2018,39(14):236-241.
[29] De Weichen, Min Zhang, Sundar Shrestha Compositional characteristics and nutritional quality of Chinese mitten crab(Eriocheir sinensis)[J].Food Chemistry,2007,103(4):1343-1349
[30]高先楚,王锡昌,顾赛麒,等.中华绒螯蟹性腺加热熟制前后挥发性成分和脂肪酸组成分析[J].现代食品科技,2014,30(9):265-274.