液相色谱—串联质谱技术用于塑料包装材料中增塑剂迁移检测的研究
摘要
本论文分为四章。在第一章中,首先介绍了近几年发展起来的应用于串联质谱仪中的软电离技术:质子转移电离技术、真空紫外灯电离源和大气压下在线直接分析电离技术。并针对不同的电离方法简单评述了其性能及应用,同时介绍了在串联质谱方面的新发展,以及串联质谱在仪器微型化方面的进展及其应用,还对串联质谱仪今后的发展作了展望。
在第二章中,详细介绍了液相色谱-串联质谱联用技术,综述了近年来液相色谱-质谱接口技术的研究进展概况,并且详细描述了液相色谱-质谱联用技术在生物制药、生物大分子、蛋白质组学、农药残留、环境污染等诸多方面的分析应用,展示了它们的发展前景。
在第三章中,详细研究了采用GC/MS和LC-MS/MS联用技术对栽培小刺猴头菌子实体中分离得到的组分进行定性和定量分析的结果,实际检测出了邻苯二甲酸二正辛酯(DNOP)和邻苯二甲酸二丁酯(DBP)二种增塑剂,这是在国内外首次详细报道了增塑剂对栽培食用菌的二次污染。另外还研究建立了有可能造成栽培食用菌被污染的9种常见增塑剂的同时检测方法。为我国相关食品安全的技术监测、预警和控制提供了必要的技术支持。
在第四章中,着重描述了所完成的科研项目——《液相色谱-串联质谱技术用于食品塑料包装材料中增塑剂迁移检测的研究》(国家质量监督检验检疫总局科研项目,课题编号:2004IK078)的内容:以我国食品塑料包装材料中广泛使用的13种增塑剂为研究对象,通过食品模拟迁移试验、储存条件、温度、时间、食品模拟物的影响及提取净化和检测方法试验等,在国内外首次研究建立了食品塑料包装材料中13种增塑剂迁移量的液相色谱-串联质谱(LC-MS/MS)检测方法和阳性确证方法,填补了我国在食品模拟迁移技术方面的空白,为对我国食品安全的监测检验、预警和控制以及破除国外技术壁垒提供了必要的技术支持。
ChapterⅠNew Developments and Applications of Mass Spectrometry
First, in Chapter one, the new developed soft ionization source which is used in tandem mass spectrometer is introduced. Proton-transfer-reaction (PTR) ionization is a high sensitive method for volatile organic compounds. Vacuum ultraviolet lamp ionization source is attractive for portable analytical instrument because of its smallness and simpleness. Desorption electrospray ionization provides better solutions for real-time , on-line and high sensitive analysis of volatile and semi-volatile organic compounds. Furthermore, it can be used in vivo sampling or living tissue surfaces. Atmospheric pressure direct analysis in real time ionization uses metastable atoms or molecules of carrier gas to produce molecular ions for analysis. Applications of these new ionization methods to various problems are also discussed. The progress in MS/MS instruments and miniaturizing instruments is reviewed and perspectives for the development of MS/MS instrument are provided.
ChapterⅡProgress and Applications in Liquid Chromatography-Mass spectrometry
Liquid chromatography-mass spectrometry method as a relatively perfect modern analytical technique embodies the superiority of LC and MS, which combines the high separation property of chromatography and the high identification property of MS. With advancements in ionization methods and instrumentation, liquid chromatography/mass spectrometry has become a powerful technology for the characterization of modern analytical chemistry. In chaper two, the research progress of the interface for liquid chromatography coupling with mass spectrometry and a brief description of the use of hyphenated LC/MS in pharmaceutica, large biomolecules, proteomics, toxic residues of pesticides, environmental pollutants and so on.
ChapterⅢDetermination of Plasticizers in the Body of Hericium Caput-Medusae by Liquid Chromatography- Tandem Mass Spectrometry
[Hericium caput-medusae(Bull.:Fr.) Pers] is valuable for being used both as medicine and food. According to literature, [Hericium caput-medusae(Bull.:Fr.) Pers] is rich in nutrients and contains various active substances, of which polysaccharide is widely studied and interested both in China and abroad. Polysaccharides of [Hericium caput-medusae(Bull.:Fr.) Pers] have been isolated from fruit-bodies or mycelium or fermented liquor by many researchers recently. Researches in medicine and pharmacology have proved that polysaccharides of [Hericium caput-medusae(Bull.:Fr.) Pers] have certain therapeutical effects on improving immunity, restraining cancer and senescence, reducing blood sugar, and so on. In this review, the latest development in studying composition, structural analysis, biological activity of polysaccharides isolated from [Hericium caput-medusae(Bull.:Fr.) Pers] and a prospect for the isolating methods were elaborated.
In this chapter, a composition extracted from the cultured body of [Hericium caput-medusae (Bull.:Fr.) Pers.] was analyzed quantitatively and qualitatively by gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. Two plasticizers, di-n-octyl o-phthalate(DOP) and di-nobutyl o-phthalate(DBP)were identified by manually mass spectrum analyzing and mass spectra bank matching, which was reported by the author for the first time. Since plastics are not inert, plasticizers might migrate into the cultured mushroom and cause contamination. A simple LC-MS/MS method was established for the determination of 9 plasticizers in cultured edible mushroom due to potential contamination. These results provided enforcement laboratories a very promising systematical control method for checking the food quality and safety.
ChapterⅣStudy of migration of plasticizers used in food plastic packaging by Liquid Chromatography Tandem Mass Spectrometry
Food contamination can result from various interactions between food and packaging materials. Packaging itself has recently been found to be a source of contamination through the migration of substances from the packaging into the food. Migration of additives, monomers and oligomers from packaging materials into food or adsorption of volatile compounds from the food by the polymer are important considerations from safety, hygienic and economic points of view. Direct contact between plastic packaging materials and food can result in migration of plasticizers from packaging materials into foodstuffs. Migration of residual printing ink solvents from packaging to food can cause off-flavours in the food and lead to a deterioration in the quality of the food products. Every day we consume foods that have been in contact with many different type of packing materials and regularly ingest hundreds of migrants. Evidence of widespread human exposure to phthalates and toxicological studies have shown that some phthalates are developmental and reproductive toxicants in animals and thus raised both scientific and public concern about the ubiquitous use of phthalates in consumer and personal care products.
In our research, some problems arised from plastic packaging are discussed from the food quality and safety point of view. Some new advances in development of migration analysis of plastic food packaging at home and abroad are introduced systematically. The progress in determination of migration of plasticizers of food plastic packaging, and various analytical techniques developed are reviewed briefly. And some problems of safety and hygienic remained in food plastic packaging faced now are discussed.
This chapter is the core content of the thesis, in which a method for determination of migration of plasticizers used in food plastic packaging to the foodstuffs by LC-MS/MS has been developed for the first time. The migration of some model contaminants from food plastic packaging was studied by taken into consideration of the influence of storage temperature, storage time, type of food simulant, using GPC coupled with SPE, LC-MS/MS and so on. A simple LC-MS/MS method was established for the determination of 13 plasticizers in food packaging with plastic. The method has shown to have good recovery (71.1%-91.3%) for various samples with different levels of spiking components (0.01-0.10mg/L). The relative standard deviations were shown to be in the range of 2.1%-8.5% for all plasticizers studied. The limits of detection were in the range of 0.002-0.03μg/L.
The developed analytical method provided a basis for takeing measures to reduce the risk in making the inspection policy for relative departments. The test method should be applicable for industry with respect to new packaging developments and should also offer enforcement laboratories a systematical control method to check the food safety of plastic packaging taken from the market.
在第二章中,详细介绍了液相色谱-串联质谱联用技术,综述了近年来液相色谱-质谱接口技术的研究进展概况,并且详细描述了液相色谱-质谱联用技术在生物制药、生物大分子、蛋白质组学、农药残留、环境污染等诸多方面的分析应用,展示了它们的发展前景。
在第三章中,详细研究了采用GC/MS和LC-MS/MS联用技术对栽培小刺猴头菌子实体中分离得到的组分进行定性和定量分析的结果,实际检测出了邻苯二甲酸二正辛酯(DNOP)和邻苯二甲酸二丁酯(DBP)二种增塑剂,这是在国内外首次详细报道了增塑剂对栽培食用菌的二次污染。另外还研究建立了有可能造成栽培食用菌被污染的9种常见增塑剂的同时检测方法。为我国相关食品安全的技术监测、预警和控制提供了必要的技术支持。
在第四章中,着重描述了所完成的科研项目——《液相色谱-串联质谱技术用于食品塑料包装材料中增塑剂迁移检测的研究》(国家质量监督检验检疫总局科研项目,课题编号:2004IK078)的内容:以我国食品塑料包装材料中广泛使用的13种增塑剂为研究对象,通过食品模拟迁移试验、储存条件、温度、时间、食品模拟物的影响及提取净化和检测方法试验等,在国内外首次研究建立了食品塑料包装材料中13种增塑剂迁移量的液相色谱-串联质谱(LC-MS/MS)检测方法和阳性确证方法,填补了我国在食品模拟迁移技术方面的空白,为对我国食品安全的监测检验、预警和控制以及破除国外技术壁垒提供了必要的技术支持。
ChapterⅠNew Developments and Applications of Mass Spectrometry
First, in Chapter one, the new developed soft ionization source which is used in tandem mass spectrometer is introduced. Proton-transfer-reaction (PTR) ionization is a high sensitive method for volatile organic compounds. Vacuum ultraviolet lamp ionization source is attractive for portable analytical instrument because of its smallness and simpleness. Desorption electrospray ionization provides better solutions for real-time , on-line and high sensitive analysis of volatile and semi-volatile organic compounds. Furthermore, it can be used in vivo sampling or living tissue surfaces. Atmospheric pressure direct analysis in real time ionization uses metastable atoms or molecules of carrier gas to produce molecular ions for analysis. Applications of these new ionization methods to various problems are also discussed. The progress in MS/MS instruments and miniaturizing instruments is reviewed and perspectives for the development of MS/MS instrument are provided.
ChapterⅡProgress and Applications in Liquid Chromatography-Mass spectrometry
Liquid chromatography-mass spectrometry method as a relatively perfect modern analytical technique embodies the superiority of LC and MS, which combines the high separation property of chromatography and the high identification property of MS. With advancements in ionization methods and instrumentation, liquid chromatography/mass spectrometry has become a powerful technology for the characterization of modern analytical chemistry. In chaper two, the research progress of the interface for liquid chromatography coupling with mass spectrometry and a brief description of the use of hyphenated LC/MS in pharmaceutica, large biomolecules, proteomics, toxic residues of pesticides, environmental pollutants and so on.
ChapterⅢDetermination of Plasticizers in the Body of Hericium Caput-Medusae by Liquid Chromatography- Tandem Mass Spectrometry
[Hericium caput-medusae(Bull.:Fr.) Pers] is valuable for being used both as medicine and food. According to literature, [Hericium caput-medusae(Bull.:Fr.) Pers] is rich in nutrients and contains various active substances, of which polysaccharide is widely studied and interested both in China and abroad. Polysaccharides of [Hericium caput-medusae(Bull.:Fr.) Pers] have been isolated from fruit-bodies or mycelium or fermented liquor by many researchers recently. Researches in medicine and pharmacology have proved that polysaccharides of [Hericium caput-medusae(Bull.:Fr.) Pers] have certain therapeutical effects on improving immunity, restraining cancer and senescence, reducing blood sugar, and so on. In this review, the latest development in studying composition, structural analysis, biological activity of polysaccharides isolated from [Hericium caput-medusae(Bull.:Fr.) Pers] and a prospect for the isolating methods were elaborated.
In this chapter, a composition extracted from the cultured body of [Hericium caput-medusae (Bull.:Fr.) Pers.] was analyzed quantitatively and qualitatively by gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. Two plasticizers, di-n-octyl o-phthalate(DOP) and di-nobutyl o-phthalate(DBP)were identified by manually mass spectrum analyzing and mass spectra bank matching, which was reported by the author for the first time. Since plastics are not inert, plasticizers might migrate into the cultured mushroom and cause contamination. A simple LC-MS/MS method was established for the determination of 9 plasticizers in cultured edible mushroom due to potential contamination. These results provided enforcement laboratories a very promising systematical control method for checking the food quality and safety.
ChapterⅣStudy of migration of plasticizers used in food plastic packaging by Liquid Chromatography Tandem Mass Spectrometry
Food contamination can result from various interactions between food and packaging materials. Packaging itself has recently been found to be a source of contamination through the migration of substances from the packaging into the food. Migration of additives, monomers and oligomers from packaging materials into food or adsorption of volatile compounds from the food by the polymer are important considerations from safety, hygienic and economic points of view. Direct contact between plastic packaging materials and food can result in migration of plasticizers from packaging materials into foodstuffs. Migration of residual printing ink solvents from packaging to food can cause off-flavours in the food and lead to a deterioration in the quality of the food products. Every day we consume foods that have been in contact with many different type of packing materials and regularly ingest hundreds of migrants. Evidence of widespread human exposure to phthalates and toxicological studies have shown that some phthalates are developmental and reproductive toxicants in animals and thus raised both scientific and public concern about the ubiquitous use of phthalates in consumer and personal care products.
In our research, some problems arised from plastic packaging are discussed from the food quality and safety point of view. Some new advances in development of migration analysis of plastic food packaging at home and abroad are introduced systematically. The progress in determination of migration of plasticizers of food plastic packaging, and various analytical techniques developed are reviewed briefly. And some problems of safety and hygienic remained in food plastic packaging faced now are discussed.
This chapter is the core content of the thesis, in which a method for determination of migration of plasticizers used in food plastic packaging to the foodstuffs by LC-MS/MS has been developed for the first time. The migration of some model contaminants from food plastic packaging was studied by taken into consideration of the influence of storage temperature, storage time, type of food simulant, using GPC coupled with SPE, LC-MS/MS and so on. A simple LC-MS/MS method was established for the determination of 13 plasticizers in food packaging with plastic. The method has shown to have good recovery (71.1%-91.3%) for various samples with different levels of spiking components (0.01-0.10mg/L). The relative standard deviations were shown to be in the range of 2.1%-8.5% for all plasticizers studied. The limits of detection were in the range of 0.002-0.03μg/L.
The developed analytical method provided a basis for takeing measures to reduce the risk in making the inspection policy for relative departments. The test method should be applicable for industry with respect to new packaging developments and should also offer enforcement laboratories a systematical control method to check the food safety of plastic packaging taken from the market.
引文
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