色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
8期
849-854
,共6页
改进的 QuEChERS%气相色谱-质谱%氟吗啉%烯酰吗啉%蔬菜%残留
改進的 QuEChERS%氣相色譜-質譜%氟嗎啉%烯酰嗎啉%蔬菜%殘留
개진적 QuEChERS%기상색보-질보%불마람%희선마람%소채%잔류
improved QuEChERS%gas chromatography-mass spectrometry(GC-MS)%flumor-ph%dimethomorph%vegetables%residue
建立了同时测定蔬菜中氟吗啉和烯酰吗啉残留的改进的 QuEChERS-气相色谱-质谱（ GC-MS）联用法。前处理过程以乙腈高速匀浆提取样品，应用改进的 QuEChERS 方法对样品进行提取、盐析和净化，并采用气相色谱-质谱联用仪在选择离子监测（SIM）模式下测定了多种蔬菜中的氟吗啉和烯酰吗啉残留量，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），流速1.1 mL / min，采用电子轰击电离源，选择监测离子氟吗啉为 m / z 285、371、165；烯酰吗啉为 m / z 301、387、165。结果表明：在优化条件下，氟吗啉和烯酰吗啉在10~1000μg / kg 范围内线性关系良好，相关系数不低于0.999，不同基质中的检出限（ S / N =3）范围为0.67~2.42μg / kg。对于生姜、番茄、胡萝卜、菠菜、甘蓝和白木耳空白样品，在10、20、100μg / kg 共3个水平下氟吗啉和烯酰吗啉的加标回收率为71％~116％，相对标准偏差（ RSD）为1.8％~14.7％。同时，本研究对蔬菜中氟吗啉和烯酰吗啉残留检测的裂解机理和基质效应进行了考察。本方法具有操作简便、快速、准确的特点，可用于蔬菜中氟吗啉和烯酰吗啉残留量的日常检测。
建立瞭同時測定蔬菜中氟嗎啉和烯酰嗎啉殘留的改進的 QuEChERS-氣相色譜-質譜（ GC-MS）聯用法。前處理過程以乙腈高速勻漿提取樣品，應用改進的 QuEChERS 方法對樣品進行提取、鹽析和淨化，併採用氣相色譜-質譜聯用儀在選擇離子鑑測（SIM）模式下測定瞭多種蔬菜中的氟嗎啉和烯酰嗎啉殘留量，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），流速1.1 mL / min，採用電子轟擊電離源，選擇鑑測離子氟嗎啉為 m / z 285、371、165；烯酰嗎啉為 m / z 301、387、165。結果錶明：在優化條件下，氟嗎啉和烯酰嗎啉在10~1000μg / kg 範圍內線性關繫良好，相關繫數不低于0.999，不同基質中的檢齣限（ S / N =3）範圍為0.67~2.42μg / kg。對于生薑、番茄、鬍蘿蔔、菠菜、甘藍和白木耳空白樣品，在10、20、100μg / kg 共3箇水平下氟嗎啉和烯酰嗎啉的加標迴收率為71％~116％，相對標準偏差（ RSD）為1.8％~14.7％。同時，本研究對蔬菜中氟嗎啉和烯酰嗎啉殘留檢測的裂解機理和基質效應進行瞭攷察。本方法具有操作簡便、快速、準確的特點，可用于蔬菜中氟嗎啉和烯酰嗎啉殘留量的日常檢測。
건립료동시측정소채중불마람화희선마람잔류적개진적 QuEChERS-기상색보-질보（ GC-MS）련용법。전처리과정이을정고속균장제취양품，응용개진적 QuEChERS 방법대양품진행제취、염석화정화，병채용기상색보-질보련용의재선택리자감측（SIM）모식하측정료다충소채중적불마람화희선마람잔류량，이기질필배표준용액외표법정량。선용 DB-5 MS 석영모세관주（30 m×0.25 mm×0.25μm），류속1.1 mL / min，채용전자굉격전리원，선택감측리자불마람위 m / z 285、371、165；희선마람위 m / z 301、387、165。결과표명：재우화조건하，불마람화희선마람재10~1000μg / kg 범위내선성관계량호，상관계수불저우0.999，불동기질중적검출한（ S / N =3）범위위0.67~2.42μg / kg。대우생강、번가、호라복、파채、감람화백목이공백양품，재10、20、100μg / kg 공3개수평하불마람화희선마람적가표회수솔위71％~116％，상대표준편차（ RSD）위1.8％~14.7％。동시，본연구대소채중불마람화희선마람잔류검측적렬해궤리화기질효응진행료고찰。본방법구유조작간편、쾌속、준학적특점，가용우소채중불마람화희선마람잔류량적일상검측。
To determine the residues of flumorph and dimethomorph in vegetables,a method was established with improved QuEChERS-gas chromatography coupled to mass spectrometry (GC-MS). With acetonitrile as the extraction solvent,the samples were pretreated with the improved QuEChERS method including extraction,salting-out and purification processes. Then all the sample extracts were analyzed with GC-MS in selected-ion monitoring(SIM)mode,and quantified by matrix-matched standard solution in external standard method. Under electron ionization conditions,the analysis was carried out with a capillary column( DB-5 MS,30 m × 0. 25 mm×0. 25 μm)at a flow rate of 1. 1 mL / min. The quantitation was performed to detect ions of m / z 285,371,165 for flumorph and m / z 301,387,165 for dimethomorph. Good lineari-ty was obtained in the range of 10-1 000 μg / kg for both pesticides with correlation coefficients greater than 0. 999. The recovery experiments were carried out by spiking blank samples of gin-ger,tomato,carrot,spinach,cabbage and tremella at the three levels of 10,20 and 100 μg / kg. For both pesticides in different matrices,the limits of detection(S / N = 3)were in the range of 0. 67-2. 42 μg / kg. The average recoveries of flumorph and dimethomorph ranged from 71% to 116% with the relative standard deviations( RSDs)in the range of 1. 8% - 14. 7% . Meanwhile, the pyrolysis mechanism and matrix effect for the determination of flumorph and dimethomorph in vegetables were investigated in this study. The method is simple,rapid and accurate,and can be used for the routine analysis of flumorph and dimethomorph in vegetables.
