农业环境科学学报
農業環境科學學報
농업배경과학학보
Journal of Agro-Environment Science
2014年
7期
1460-1464
,共5页
杨锚%王淼%佘永新%李腾飞%王静%王珊珊%金芬%金茂俊%邵华%曹维强
楊錨%王淼%佘永新%李騰飛%王靜%王珊珊%金芬%金茂俊%邵華%曹維彊
양묘%왕묘%사영신%리등비%왕정%왕산산%금분%금무준%소화%조유강
辛基酚%壬基酚%短链壬基酚聚氧乙烯醚类%高效液相色谱串联质谱法
辛基酚%壬基酚%短鏈壬基酚聚氧乙烯醚類%高效液相色譜串聯質譜法
신기분%임기분%단련임기분취양을희미류%고효액상색보천련질보법
octylphenol%nonylphenol%short chain nonylphenol polyethoxylates%LC-MS/MS
建立了环境内分泌干扰物辛基酚、壬基酚及短链壬基酚聚氧乙烯醚降解产物的高效液相色谱串联质谱分析方法。选择易受环境污染的玉米、白菜等农产品及目标物可能迁移到环境中的食品包装材料为研究对象,经过液液萃取、浓缩,乙腈甲苯(3:1)溶液溶解,经ENVITM CarbⅡ/PSA氨基固相萃取柱净化,甲醇-二氯甲烷(4:3)溶液为洗脱液。采用Agilent ZORBAX RX-C18柱,以甲醇:10 mmol·L-1乙酸铵(9:1)为流动相,梯度洗脱分离后,在LC-MS/MS多反应监测模式下正负离子同时扫描进行定性与定量分析。结果表明,该方法对辛基酚、壬基酚、壬基酚一氧乙烯醚和壬基酚二氧乙烯醚的检出限分别为0.03、0.6、1.6、0.03μg·kg-1,在不同基质中添加浓度为0.5~5μg·kg-1的四种物质平均回收率在62%~113%之间。对实际样品进行检测时,在蔬菜和粮食作物及其包装材料中分别检测到不同含量的上述物质,表明该方法准确、快速、灵敏度高,可用于农产品和食品包装材料中该类物质的监控。
建立瞭環境內分泌榦擾物辛基酚、壬基酚及短鏈壬基酚聚氧乙烯醚降解產物的高效液相色譜串聯質譜分析方法。選擇易受環境汙染的玉米、白菜等農產品及目標物可能遷移到環境中的食品包裝材料為研究對象,經過液液萃取、濃縮,乙腈甲苯(3:1)溶液溶解,經ENVITM CarbⅡ/PSA氨基固相萃取柱淨化,甲醇-二氯甲烷(4:3)溶液為洗脫液。採用Agilent ZORBAX RX-C18柱,以甲醇:10 mmol·L-1乙痠銨(9:1)為流動相,梯度洗脫分離後,在LC-MS/MS多反應鑑測模式下正負離子同時掃描進行定性與定量分析。結果錶明,該方法對辛基酚、壬基酚、壬基酚一氧乙烯醚和壬基酚二氧乙烯醚的檢齣限分彆為0.03、0.6、1.6、0.03μg·kg-1,在不同基質中添加濃度為0.5~5μg·kg-1的四種物質平均迴收率在62%~113%之間。對實際樣品進行檢測時,在蔬菜和糧食作物及其包裝材料中分彆檢測到不同含量的上述物質,錶明該方法準確、快速、靈敏度高,可用于農產品和食品包裝材料中該類物質的鑑控。
건립료배경내분비간우물신기분、임기분급단련임기분취양을희미강해산물적고효액상색보천련질보분석방법。선택역수배경오염적옥미、백채등농산품급목표물가능천이도배경중적식품포장재료위연구대상,경과액액췌취、농축,을정갑분(3:1)용액용해,경ENVITM CarbⅡ/PSA안기고상췌취주정화,갑순-이록갑완(4:3)용액위세탈액。채용Agilent ZORBAX RX-C18주,이갑순:10 mmol·L-1을산안(9:1)위류동상,제도세탈분리후,재LC-MS/MS다반응감측모식하정부리자동시소묘진행정성여정량분석。결과표명,해방법대신기분、임기분、임기분일양을희미화임기분이양을희미적검출한분별위0.03、0.6、1.6、0.03μg·kg-1,재불동기질중첨가농도위0.5~5μg·kg-1적사충물질평균회수솔재62%~113%지간。대실제양품진행검측시,재소채화양식작물급기포장재료중분별검측도불동함량적상술물질,표명해방법준학、쾌속、령민도고,가용우농산품화식품포장재료중해류물질적감공。
A novel method was established for simultaneous determination of octylpehenol(OP), nonylphenol(NP), nonylphenol mo-noethoxylates(NPEO1)and nonylphenol diethoxylates(NPEO2)in agro-products and food packages with liquid chromatography-tandem quadrupole mass spectrometry(HPLC- MS/MS). These analytes were extracted from vegetables, crops and food packaging materials with acetonitrile and toluene solution. The extracts were cleaned using solid phase extraction with graphitized carbon black tandem and primary secondary amine(PSA)cartridges. LC-MS/MS was utilized for simultaneous analysis of OP, NP, NPEO1 and NPEO2. After chromatograph-ic separation on Agilent ZORBAX RX-C18 column with methanol-10 mmol·L-1 ammonium acetate gradient elution, qualitative and quanti-tative analyses were carried out under the simultaneous scanning models of positive and negative. The average recoveries for agro-products and food packaging materials at spiked levels of 0.5~5μg·kg-1 were from 62%to 113%. The limit of detection(LOD)of OP, NP, NPEO1 and NPEO2 was 0.03μg·kg-1, 0.6μg·kg-1, 1.6μg·kg-1 and 0.03μg·kg-1, respectively. This method is accurate, rapid, and sensitive, and could be used for quick and routine determination of OP, NP, NPEO1 and NPEO2 in agro-products and food packages.