芝麻中塑化剂含量及其在制油过程中的迁移规律
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摘要
通过对不同地区20个芝麻样品中邻苯二甲酸酯(phthalatic acid esters,PAEs)组分含量的检测分析,以及芝麻中PAEs在制油过程向毛油中迁移规律研究,明确芝麻油生产中原料和制油工艺对芝麻油PAEs风险的影响,以便准确制定PAEs风险防范和控制技术,确保并提升芝麻油的品质安全。结果表明,20个芝麻样品均不同程度检出PAEs,国标限量控制的邻苯二甲酸二丁酯(dibutyl phthalate,DBP)、邻苯二甲酸二(2-乙基)己酯(di(2-ethtlhexyl) phthalate,DEHP)、邻苯二甲酸二异壬酯(diisononyl ortho-phthalate,DINP)的检出率为100%,3种组分和8种塑化剂总含量(Σ8PAEs)分别为0.040～0.337、0.085～1.971、0.343～0.806 mg/kg和0.209～2.828 mg/kg,平均值分别为0.137、0.560、0.559 mg/kg和1.165 mg/kg。对照国标DBP≤0.3 mg/kg、DEHP≤1.5 mg/kg、DINP≤9.0 mg/kg的限量指标,DEHP超标率为5%,DBP超标率为10%。芝麻原料中的PAEs随着制油过程向毛油中迁移富集,DBP、DEHP、DINP和Σ8PAEs在压榨毛油中的含量分别是芝麻中的1.16、1.03、1.11倍和1.07倍,在浸出毛油中的含量分别是芝麻中的1.49、1.27、1.24倍和1.33倍,脱皮芝麻毛油中PAEs含量比整籽芝麻毛油含量降低约20%,浸出毛油中PAEs含量约是压榨毛油1.2倍。
In this paper, the contents of phthalic acid esters(PAEs) in 20 sesame seed samples collected from different areas were analyzed. The migration of PAEs into crude sesame oil during oil processing was studied. The effects of raw materials and processing technologies on PAEs migration into sesame oil were clarified in order to develop technologies for accurately preventing and controlling the risk of PAEs migration and consequently to ensure and enhance the quality and safety of sesame oil. The results showed that all samples were found to contain PAEs. Dibutyl phthalate(DBP),di(2-ethtlhexyl) phthalate(DEHP) and diisononyl ortho-phthalate(DINP), with limits set for all of them(DBP ≤ 0.3 mg/kg,DEHP ≤ 1.5 mg/kg, and DINP ≤ 9.0 mg/kg) in the Chinese national standard, were detected in 100% of the samples in the range of 0.040–0.337, 0.085–1.971 and 0.343–0.806 mg/kg with an average of 0.137, 0.560 and 0.559 mg/kg, respectively.A total of 8ΣPAEs were detected in all samples in the range of 0.209–2.828 mg/kg with an average of 1.165 mg/kg. Five and10 percent of the samples exceeded the national standard limits for DEHP and DBP, respectively. The PAEs were gradually migrated from sesame into crude oil and accumulated during oil production. The contents of DBP, DEHP and DINP and total PAEs content of the crude pressed oil were 1.16, 1.03, 1.11 and 1.07 times higher than those of sesame seeds, respectively.The solvent extracted oil contained 1.49, 1.27, 1.24 and 1.33 times more DBP, DEHP and DINP and total PAEs than sesame seeds, respectively. The content of PAEs in the peeled sesame oil was about 20% lower than that in the whole sesame oil,and the PAEs content in the extracted oil was about 1.2 times higher than that in the pressed oil.
In this paper, the contents of phthalic acid esters(PAEs) in 20 sesame seed samples collected from different areas were analyzed. The migration of PAEs into crude sesame oil during oil processing was studied. The effects of raw materials and processing technologies on PAEs migration into sesame oil were clarified in order to develop technologies for accurately preventing and controlling the risk of PAEs migration and consequently to ensure and enhance the quality and safety of sesame oil. The results showed that all samples were found to contain PAEs. Dibutyl phthalate(DBP),di(2-ethtlhexyl) phthalate(DEHP) and diisononyl ortho-phthalate(DINP), with limits set for all of them(DBP ≤ 0.3 mg/kg,DEHP ≤ 1.5 mg/kg, and DINP ≤ 9.0 mg/kg) in the Chinese national standard, were detected in 100% of the samples in the range of 0.040–0.337, 0.085–1.971 and 0.343–0.806 mg/kg with an average of 0.137, 0.560 and 0.559 mg/kg, respectively.A total of 8ΣPAEs were detected in all samples in the range of 0.209–2.828 mg/kg with an average of 1.165 mg/kg. Five and10 percent of the samples exceeded the national standard limits for DEHP and DBP, respectively. The PAEs were gradually migrated from sesame into crude oil and accumulated during oil production. The contents of DBP, DEHP and DINP and total PAEs content of the crude pressed oil were 1.16, 1.03, 1.11 and 1.07 times higher than those of sesame seeds, respectively.The solvent extracted oil contained 1.49, 1.27, 1.24 and 1.33 times more DBP, DEHP and DINP and total PAEs than sesame seeds, respectively. The content of PAEs in the peeled sesame oil was about 20% lower than that in the whole sesame oil,and the PAEs content in the extracted oil was about 1.2 times higher than that in the pressed oil.
引文
[1]宋雪英,崔小维,李嘉康,等.邻苯二甲酸酯类塑化剂的土壤生态毒理学研究进展[J].生态环境学报,2016,25(11):1885-1890.DOI:10.16258/j.cnki.1674-5906.2016.11.022.
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[4]XU C K,WANG X H,TANG S B.Effects of di-(2-ethylhexyl)phthalate on rat ovarian function[J].Journal of Medical Biochemistry,2011,30:309-316.DOI:10.2478/v10011-011-0026-2.
[5]KONSTANTIN S,IRINA S,OLLE S.Inhibitory effects of monoethylhexyl phthalate on steroidogenesis in immature and adultrat leydig in vitro[J].Reproductive Toxicology,2008,25(4):485-490.DOI:10.1016/j.reprotox.2008.05.057.
[6]FU X W,DU Q Z.Uptake of di-(2-ethylhexyl)phthalate of vegetables from plastic film greenhouses[J].Agricultural and Food Chemistry,2011,59(21):11585-11588.DOI:10.1021/jf203502e.
[7]王绪强.植物累积有机污染物DEHP能力及其特异性研究[D].杭州:浙江工商大学,2009.
[8]曾巧云,莫测辉,蔡全英,等.菜心对邻苯二甲酸酯(PAEs)吸收途径的初步研究[J].农业工程学报,2005,21(8):137-141.DOI:10.3321/j.issn:1002-6819.2005.08.030.
[9]王瑞元,金青哲,安骏.塑化剂与粮油制品的安全[J].中国油脂,2013,38(4):1-4.DOI:10.3969/j.issn.1003-7969.2013.04.001.
[10]张明明.植物油料和食用油脂中邻苯二甲酸酯类物质(PAEs)含量的研究[D].郑州:河南工业大学,2014.
[11]SHI L K,ZHANG M M,LIU Y L.Concentration and survey of phthalic acid esters in edible vegetable oils and oilseeds by gas chromatography-mass spectrometry in China[J].Food Control,2016,68:118-123.DOI:10.1016/j.foodcont.2016.03.027.
[12]梁少华,汪学德,魏安池,等.芝麻加工贸易现状及技术需求的调研[J].中国油脂,2009,34(8):10-15.DOI:10.3321/j.issn:1003-7969.2009.08.003.
[13]国家卫生和计划生育委员会,国家食品药品监督管理总局.食品中邻苯二甲酸酯的测定:GB 5009.271-2016[S].北京:中国标准出版社,2016.
[14]胡爱鹏,刘玉兰,张明明,等.气相色谱-质谱联用法直接测定植物油料中邻苯二甲酸酯类塑化剂[J].食品科学,2016,37(18):146-151.DOI:10.7506/spkx1002-6630-201618024.
[15]张明明,刘玉兰,马宇翔,等.固相萃取-气相色谱-质谱法测定食用油中7种邻苯二甲酸酯类塑化剂[J].中国油脂,2015,40(2):56-60.
[16]卫生部.卫生部办公厅关于通报食品及食品添加剂中邻苯二甲酸酯类物质最大残留量的函(卫办监督函[2011]551号)[EB/OL].http://www.nhfpc.gov.cn/sps/s3594/201211/2b4831f001a740a48086f ad152117286.shtml.2011-6-13.
[17]HU A P,LIU Y L,SHI L K.Widespread occurrence of phthalic acid esters in raw oilseeds in China used for edible vegetable oil production[J].Food Additives&Contaminants:Part A,2016,33(9):1421-1427.DOI:10.1080/19440049.2016.1222631.
[18]杨金强.食用油脂加工中PAEs变化规律的研究[D].郑州:河南工业大学,2016.
[19]刘庆,杨红军,石衍玺,等.环境中邻苯二甲酸酯类(PAEs)污染物研究进展[J].中国生态农业学报,2012,20(8):968-975.
[20]莫测辉,蔡全英,吴启堂,等.我国城市污泥中邻苯二甲酸酯的研究[J].中国环境科学,2001,21(4):362-366.DOI:10.3321/j.issn:1000-6923.2001.04.019.
[21]王春兰.浅析地膜覆盖对环境污染的防治与建议[J].农业与技术,2013,33(7):18-25.DOI:10.3969/j.issn.1671-962X.2013.07.017.
[22]巩余禾,赵文良.环境水体中邻苯二甲酸酯类化合物的方法研究[J].中国卫生检验杂志,2009,19(11):2468-2469.
[23]催明明,王凯荣,王琳琳,等.山东省花生主产区土壤和花生籽粒中邻苯二甲酸酯的分布特征[J].应用生态学报,2013,24(12):3523-3530.DOI:10.13287/j.1001-9332.2013.0589.
[24]曹莹,陈莎,王晓伟,等.环境中邻苯二甲酸酯类化合物的分析测定[J].环境与健康,2007,24(7):546-549.DOI:10.3969/j.issn.1001-5914.2007.07.033.
[25]KONG S F,JI Y Q,LIU L L,et al.Diversities of phthalate esters in suburban agricultural soils and wasteland soil appeared with urbanization in China[J].Environmental Pollution,2012,170:161-168.DOI:10.1016/j.envpol.2012.06.017.
[26]国家卫生和计划生育委员会.食用植物油料:GB 19641-2015[S].北京:中国标准出版社,2015.
[27]柳春红,孙远明,杨艺超,等.邻苯二甲酸酯类增塑剂的污染及暴露评估现状[J].现代食品科技,2012,28(3):339-341;338.DOI:10.3969/j.issn.1673-9078.2012.03.025.
[28]邹翀,尤梦圆,刘金勇,等.食用油中邻苯二甲酸酯类物质的来源分析及预防措施[J].中国粮油学报,2014,29(7):102-107.
[29]高锦鸿,梅鸿献,刘艳阳,等.产地及籽粒外观品质对芝麻木酚素含量的影响[J].华北农学报,2015,30(2):191-197.DOI:10.7668/hbnxb.2015.02.033.
[30]胡爱鹏.植物油料及加工产物中PAEs的研究[D].郑州:河南工业大学,2017.
[31]刘玉兰,杨金强,张明明,等.分子蒸馏法脱除油脂中塑化剂效果的研究[J].粮食与油脂,2016,29(2):19-22.DOI:10.3969/j.issn.1008-9578.2016.02.005.
[32]刘玉兰,张明明,杨金强.水蒸汽蒸馏法对油脂中DBP和DEHP脱除效果的研究[J].现代食品科技,2017(5):1-8.DOI:10.13982/j.mfst.1673-9078.2017.5.028.
[33]刘平香,陈红平,张明露,等.茶叶中邻苯二甲酸酯污染水平及检测技术研究进展[J].浙江农业科学,2015,56(11):1796-1804.DOI:10.16178/j.issn.0528-9017.20151129.
[2]EMA M,MIYAWAKI E.Adverse effects on development of the reproductive system in male offspring of rats given monobutyl phthalate,a metabolite of dibutyl phthalate,during late pregnancy[J].Reproductive Toxicology,2001,15:189-194.DOI:10.1016/S0890-6238(01)00111-3.
[3]ARCAKI F A,COSTA C,IMPERATORE C,et al.Oral toxicity of bis(2-ethylhexyl)phthalate during pregnancy and suckling in the Long-Evans rat[J].Food and Chemical Toxicology,1998,36(11):963-970.DOI:10.1016/S0278-6915(98)00065-9.
[4]XU C K,WANG X H,TANG S B.Effects of di-(2-ethylhexyl)phthalate on rat ovarian function[J].Journal of Medical Biochemistry,2011,30:309-316.DOI:10.2478/v10011-011-0026-2.
[5]KONSTANTIN S,IRINA S,OLLE S.Inhibitory effects of monoethylhexyl phthalate on steroidogenesis in immature and adultrat leydig in vitro[J].Reproductive Toxicology,2008,25(4):485-490.DOI:10.1016/j.reprotox.2008.05.057.
[6]FU X W,DU Q Z.Uptake of di-(2-ethylhexyl)phthalate of vegetables from plastic film greenhouses[J].Agricultural and Food Chemistry,2011,59(21):11585-11588.DOI:10.1021/jf203502e.
[7]王绪强.植物累积有机污染物DEHP能力及其特异性研究[D].杭州:浙江工商大学,2009.
[8]曾巧云,莫测辉,蔡全英,等.菜心对邻苯二甲酸酯(PAEs)吸收途径的初步研究[J].农业工程学报,2005,21(8):137-141.DOI:10.3321/j.issn:1002-6819.2005.08.030.
[9]王瑞元,金青哲,安骏.塑化剂与粮油制品的安全[J].中国油脂,2013,38(4):1-4.DOI:10.3969/j.issn.1003-7969.2013.04.001.
[10]张明明.植物油料和食用油脂中邻苯二甲酸酯类物质(PAEs)含量的研究[D].郑州:河南工业大学,2014.
[11]SHI L K,ZHANG M M,LIU Y L.Concentration and survey of phthalic acid esters in edible vegetable oils and oilseeds by gas chromatography-mass spectrometry in China[J].Food Control,2016,68:118-123.DOI:10.1016/j.foodcont.2016.03.027.
[12]梁少华,汪学德,魏安池,等.芝麻加工贸易现状及技术需求的调研[J].中国油脂,2009,34(8):10-15.DOI:10.3321/j.issn:1003-7969.2009.08.003.
[13]国家卫生和计划生育委员会,国家食品药品监督管理总局.食品中邻苯二甲酸酯的测定:GB 5009.271-2016[S].北京:中国标准出版社,2016.
[14]胡爱鹏,刘玉兰,张明明,等.气相色谱-质谱联用法直接测定植物油料中邻苯二甲酸酯类塑化剂[J].食品科学,2016,37(18):146-151.DOI:10.7506/spkx1002-6630-201618024.
[15]张明明,刘玉兰,马宇翔,等.固相萃取-气相色谱-质谱法测定食用油中7种邻苯二甲酸酯类塑化剂[J].中国油脂,2015,40(2):56-60.
[16]卫生部.卫生部办公厅关于通报食品及食品添加剂中邻苯二甲酸酯类物质最大残留量的函(卫办监督函[2011]551号)[EB/OL].http://www.nhfpc.gov.cn/sps/s3594/201211/2b4831f001a740a48086f ad152117286.shtml.2011-6-13.
[17]HU A P,LIU Y L,SHI L K.Widespread occurrence of phthalic acid esters in raw oilseeds in China used for edible vegetable oil production[J].Food Additives&Contaminants:Part A,2016,33(9):1421-1427.DOI:10.1080/19440049.2016.1222631.
[18]杨金强.食用油脂加工中PAEs变化规律的研究[D].郑州:河南工业大学,2016.
[19]刘庆,杨红军,石衍玺,等.环境中邻苯二甲酸酯类(PAEs)污染物研究进展[J].中国生态农业学报,2012,20(8):968-975.
[20]莫测辉,蔡全英,吴启堂,等.我国城市污泥中邻苯二甲酸酯的研究[J].中国环境科学,2001,21(4):362-366.DOI:10.3321/j.issn:1000-6923.2001.04.019.
[21]王春兰.浅析地膜覆盖对环境污染的防治与建议[J].农业与技术,2013,33(7):18-25.DOI:10.3969/j.issn.1671-962X.2013.07.017.
[22]巩余禾,赵文良.环境水体中邻苯二甲酸酯类化合物的方法研究[J].中国卫生检验杂志,2009,19(11):2468-2469.
[23]催明明,王凯荣,王琳琳,等.山东省花生主产区土壤和花生籽粒中邻苯二甲酸酯的分布特征[J].应用生态学报,2013,24(12):3523-3530.DOI:10.13287/j.1001-9332.2013.0589.
[24]曹莹,陈莎,王晓伟,等.环境中邻苯二甲酸酯类化合物的分析测定[J].环境与健康,2007,24(7):546-549.DOI:10.3969/j.issn.1001-5914.2007.07.033.
[25]KONG S F,JI Y Q,LIU L L,et al.Diversities of phthalate esters in suburban agricultural soils and wasteland soil appeared with urbanization in China[J].Environmental Pollution,2012,170:161-168.DOI:10.1016/j.envpol.2012.06.017.
[26]国家卫生和计划生育委员会.食用植物油料:GB 19641-2015[S].北京:中国标准出版社,2015.
[27]柳春红,孙远明,杨艺超,等.邻苯二甲酸酯类增塑剂的污染及暴露评估现状[J].现代食品科技,2012,28(3):339-341;338.DOI:10.3969/j.issn.1673-9078.2012.03.025.
[28]邹翀,尤梦圆,刘金勇,等.食用油中邻苯二甲酸酯类物质的来源分析及预防措施[J].中国粮油学报,2014,29(7):102-107.
[29]高锦鸿,梅鸿献,刘艳阳,等.产地及籽粒外观品质对芝麻木酚素含量的影响[J].华北农学报,2015,30(2):191-197.DOI:10.7668/hbnxb.2015.02.033.
[30]胡爱鹏.植物油料及加工产物中PAEs的研究[D].郑州:河南工业大学,2017.
[31]刘玉兰,杨金强,张明明,等.分子蒸馏法脱除油脂中塑化剂效果的研究[J].粮食与油脂,2016,29(2):19-22.DOI:10.3969/j.issn.1008-9578.2016.02.005.
[32]刘玉兰,张明明,杨金强.水蒸汽蒸馏法对油脂中DBP和DEHP脱除效果的研究[J].现代食品科技,2017(5):1-8.DOI:10.13982/j.mfst.1673-9078.2017.5.028.
[33]刘平香,陈红平,张明露,等.茶叶中邻苯二甲酸酯污染水平及检测技术研究进展[J].浙江农业科学,2015,56(11):1796-1804.DOI:10.16178/j.issn.0528-9017.20151129.