色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
3期
309-313
,共5页
丁立平%蔡春平%林永辉%吴文凡%方祥
丁立平%蔡春平%林永輝%吳文凡%方祥
정립평%채춘평%림영휘%오문범%방상
多重吸附同步净化%气相色谱-质谱%二甲苯麝香%酮麝香%水产品
多重吸附同步淨化%氣相色譜-質譜%二甲苯麝香%酮麝香%水產品
다중흡부동보정화%기상색보-질보%이갑분사향%동사향%수산품
multiple adsorption synchronous purification( MASP)%gas chromatography-mass spectrometry(GC-MS)%musk xylene%musk ketone%aquatic products
为了考察水产品中二甲苯麝香和酮麝香的残留量,建立了水产品中痕量二甲苯麝香和酮麝香测定的多重吸附同步净化(MASP)-气相色谱-质谱联用法(GC-MS)。以乙腈高速匀浆提取样品,应用 MASP 方法对样品同时进行提取、盐析和净化,并采用 GC-MS 在选择离子监测( SIM)模式下测定水产品中的痕量二甲苯麝香和酮麝香,以基质匹配标准溶液外标法定量。选用 DB-5 MS 石英毛细管柱(30 m×0.25 mm×0.25μm),采用电子轰击电离源,二甲苯麝香的选择监测离子为 m / z 282、297、265,酮麝香为 m / z 279、294、191。结果表明:在优化条件下,二甲苯麝香和酮麝香在1~100μg / kg 范围内线性良好,相关系数不低于0.999,检出限(S / N =3)为0.30μg / kg。明虾、花蛤和鳗鱼空白样品中1.0、2.0、10.0μg / kg 3个添加水平下二甲苯麝香和酮麝香的加标回收率为79%~104%,相对标准偏差(RSD)为1.6%~13.3%。本方法具有操作简便、快速、准确的特点,可用于水产品中痕量二甲苯麝香和酮麝香的日常检测。
為瞭攷察水產品中二甲苯麝香和酮麝香的殘留量,建立瞭水產品中痕量二甲苯麝香和酮麝香測定的多重吸附同步淨化(MASP)-氣相色譜-質譜聯用法(GC-MS)。以乙腈高速勻漿提取樣品,應用 MASP 方法對樣品同時進行提取、鹽析和淨化,併採用 GC-MS 在選擇離子鑑測( SIM)模式下測定水產品中的痕量二甲苯麝香和酮麝香,以基質匹配標準溶液外標法定量。選用 DB-5 MS 石英毛細管柱(30 m×0.25 mm×0.25μm),採用電子轟擊電離源,二甲苯麝香的選擇鑑測離子為 m / z 282、297、265,酮麝香為 m / z 279、294、191。結果錶明:在優化條件下,二甲苯麝香和酮麝香在1~100μg / kg 範圍內線性良好,相關繫數不低于0.999,檢齣限(S / N =3)為0.30μg / kg。明蝦、花蛤和鰻魚空白樣品中1.0、2.0、10.0μg / kg 3箇添加水平下二甲苯麝香和酮麝香的加標迴收率為79%~104%,相對標準偏差(RSD)為1.6%~13.3%。本方法具有操作簡便、快速、準確的特點,可用于水產品中痕量二甲苯麝香和酮麝香的日常檢測。
위료고찰수산품중이갑분사향화동사향적잔류량,건립료수산품중흔량이갑분사향화동사향측정적다중흡부동보정화(MASP)-기상색보-질보련용법(GC-MS)。이을정고속균장제취양품,응용 MASP 방법대양품동시진행제취、염석화정화,병채용 GC-MS 재선택리자감측( SIM)모식하측정수산품중적흔량이갑분사향화동사향,이기질필배표준용액외표법정량。선용 DB-5 MS 석영모세관주(30 m×0.25 mm×0.25μm),채용전자굉격전리원,이갑분사향적선택감측리자위 m / z 282、297、265,동사향위 m / z 279、294、191。결과표명:재우화조건하,이갑분사향화동사향재1~100μg / kg 범위내선성량호,상관계수불저우0.999,검출한(S / N =3)위0.30μg / kg。명하、화합화만어공백양품중1.0、2.0、10.0μg / kg 3개첨가수평하이갑분사향화동사향적가표회수솔위79%~104%,상대표준편차(RSD)위1.6%~13.3%。본방법구유조작간편、쾌속、준학적특점,가용우수산품중흔량이갑분사향화동사향적일상검측。
In order to investigate the residues of musk xylene and musk ketone in aquatic prod-ucts,a method was established for the determination of the trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification( MASP)-gas chro-matography-mass spectrometry(GC-MS). After extracted with acetonitrile,the samples were pretreated using MASP method including extraction,salting-out and purification processes, analyzed with GC-MS in the selected ion monitoring( SIM ) mode,and then quantified by matrix-matched standard solution in external standard method. The analysis was carried out with a capillary column(DB-5 MS,30 m×0. 25 mm×0. 25 μm)under electron ionization condi-tions. The quantification was performed using monitoring ions of m / z 282,297,265 for musk xylene and m / z 279,294,191 for musk ketone. The results showed good linearity in the range of 1-100 μg / kg for musk xylene and musk ketone with the correlation coefficients not less than 0. 999,and the limits of detection( S / N = 3)of 0. 30 μg / kg. The average recoveries of musk xylene and musk ketone spiked in prawn,clam and sea eel blank samples at three spiked levels of 1. 0,2. 0 and 10. 0 μg / kg ranged from 79% to 104% and the RSDs were in the range of 1. 6%-13. 3% . The method is simple,rapid and accurate,and can be used for the routine analysis of musk xylene and musk ketone in aquatic products.