福建分析测试
福建分析測試
복건분석측시
FUJIAN ANALYSIS & TESTING
2015年
1期
1-5
,共5页
陈旻实%林星辉%郑洁%郑思远%陈佳敏%张灵玲
陳旻實%林星輝%鄭潔%鄭思遠%陳佳敏%張靈玲
진민실%림성휘%정길%정사원%진가민%장령령
邻苯基苯酚%噻苯咪唑%联苯%抑霉唑%食品接触产品%气相色谱质谱联用%迁移
鄰苯基苯酚%噻苯咪唑%聯苯%抑黴唑%食品接觸產品%氣相色譜質譜聯用%遷移
린분기분분%새분미서%련분%억매서%식품접촉산품%기상색보질보련용%천이
Ortho-phenylphenol%Thiabendazole%Biphenyl%Imazalil%Food contact materials and articles,Gas chromatogra-phy-mass spectrometry%Migration test
建立了气相色谱质谱联用技术同时测定邻苯基苯酚(OPP)、噻苯咪唑(TBZ)、联苯(DP)及抑霉唑(IMZ)迁移量的方法。样品分别采用水、4%乙酸、20%乙醇、50%乙醇作为食品模拟物,在特定条件下浸泡提取。浸泡液运用固相萃取技术净化提纯后过0.45μm 微孔薄膜,在微极性柱上进行分离,质谱检测,外标法定量分析。优化条件下, OPP、TBZ、DP、IMZ在2-800μg/L浓度范围内与其峰面积线性良好,定量限分别为3、5、2和5μg/L(S/N=10)。在3个浓度水平进行添加实验,OPP、TBZ、DP、IMZ的平均回收率在70.4-112%之间,重复性精密度在1.78-6.72%(n=6)之间。结果表明,本方法操作简单快速、重现性好、准确度高。
建立瞭氣相色譜質譜聯用技術同時測定鄰苯基苯酚(OPP)、噻苯咪唑(TBZ)、聯苯(DP)及抑黴唑(IMZ)遷移量的方法。樣品分彆採用水、4%乙痠、20%乙醇、50%乙醇作為食品模擬物,在特定條件下浸泡提取。浸泡液運用固相萃取技術淨化提純後過0.45μm 微孔薄膜,在微極性柱上進行分離,質譜檢測,外標法定量分析。優化條件下, OPP、TBZ、DP、IMZ在2-800μg/L濃度範圍內與其峰麵積線性良好,定量限分彆為3、5、2和5μg/L(S/N=10)。在3箇濃度水平進行添加實驗,OPP、TBZ、DP、IMZ的平均迴收率在70.4-112%之間,重複性精密度在1.78-6.72%(n=6)之間。結果錶明,本方法操作簡單快速、重現性好、準確度高。
건립료기상색보질보련용기술동시측정린분기분분(OPP)、새분미서(TBZ)、련분(DP)급억매서(IMZ)천이량적방법。양품분별채용수、4%을산、20%을순、50%을순작위식품모의물,재특정조건하침포제취。침포액운용고상췌취기술정화제순후과0.45μm 미공박막,재미겁성주상진행분리,질보검측,외표법정량분석。우화조건하, OPP、TBZ、DP、IMZ재2-800μg/L농도범위내여기봉면적선성량호,정량한분별위3、5、2화5μg/L(S/N=10)。재3개농도수평진행첨가실험,OPP、TBZ、DP、IMZ적평균회수솔재70.4-112%지간,중복성정밀도재1.78-6.72%(n=6)지간。결과표명,본방법조작간단쾌속、중현성호、준학도고。
A novel SPE-GC-MS method of determination of ortho-phenylphenol,thiabendazole,biphenyl and imazalil in food stimulants was developed. Samples were immersed in stimulants(H2O,4% acetic acid,20% ethanol and 50% etha?nol),and kept in incubator at 60℃ in a duration of 2h. The immersed solutions were purified by SPE micro column before the penetration through a 0.45-μm microporous membrane. And then the purified solutions were injected into GC-MS polar column. With external standard method,the values were gotten by MS detection. Under the optimum conditions,the cali?bration curves were linear from 2 to 800 μg/L with LOQs(S/N = 10)of 3,5,2 and 5 μg/L for OPP,TBZ,DB,IMZ,re?spectively. The method provided recoveries of 70.4 % -112 % in three kinds of spiked concentrations,and the RSD of were between 1.78 % and 6.72 %. The satisfied experimental results indicated that the proposed method can be directly used for determination of OPP,TBZ,DB and IMZ in food stimulants conveniently,rapidly,reproducibly and accurately.