检验检疫学刊
檢驗檢疫學刊
검험검역학간
INSPECTION AND QUARANTINE SCIENCE
2014年
4期
55-57,32
,共4页
张鑫鑫%杨燕强%赵发宝%秦军
張鑫鑫%楊燕彊%趙髮寶%秦軍
장흠흠%양연강%조발보%진군
有机磷农药残留%基质效应%气相色谱
有機燐農藥殘留%基質效應%氣相色譜
유궤린농약잔류%기질효응%기상색보
Organ-Phosphorus Pesticide Residues%Effect on Matrix%Gas Chromatography
建立同时测定玉米蛋白粉中高毒有机磷农药甲胺磷、甲拌磷、毒死蜱、甲基嘧啶磷残留量的气相色谱分析方法。样品经乙酸乙酯提取,用中性氧化铝和活性炭作为净化剂,采用DB-1型毛细管色谱柱及FPD检测器检测,并对检测中的基质效应现象进行研究。利用阴性样品空白基质配置标准曲线进行定量分析时,发现不同农药在玉米蛋白粉中的基质效应程度不同,其中个别农药在基质中受到保护。本方法避免了保留时间漂移、检测结果假阳性和峰型拖尾的问题,结果表明,测定4种有机磷农药残留量的线性范围均为0.1-0.5mg/L,相关系数为0.9974-0.9989,检出限为0.001-0.009mg/L,3个水平的加标回收率为80.20%-92.40%,相对标准偏差为0.70%-5.47%。
建立同時測定玉米蛋白粉中高毒有機燐農藥甲胺燐、甲拌燐、毒死蜱、甲基嘧啶燐殘留量的氣相色譜分析方法。樣品經乙痠乙酯提取,用中性氧化鋁和活性炭作為淨化劑,採用DB-1型毛細管色譜柱及FPD檢測器檢測,併對檢測中的基質效應現象進行研究。利用陰性樣品空白基質配置標準麯線進行定量分析時,髮現不同農藥在玉米蛋白粉中的基質效應程度不同,其中箇彆農藥在基質中受到保護。本方法避免瞭保留時間漂移、檢測結果假暘性和峰型拖尾的問題,結果錶明,測定4種有機燐農藥殘留量的線性範圍均為0.1-0.5mg/L,相關繫數為0.9974-0.9989,檢齣限為0.001-0.009mg/L,3箇水平的加標迴收率為80.20%-92.40%,相對標準偏差為0.70%-5.47%。
건립동시측정옥미단백분중고독유궤린농약갑알린、갑반린、독사비、갑기밀정린잔류량적기상색보분석방법。양품경을산을지제취,용중성양화려화활성탄작위정화제,채용DB-1형모세관색보주급FPD검측기검측,병대검측중적기질효응현상진행연구。이용음성양품공백기질배치표준곡선진행정량분석시,발현불동농약재옥미단백분중적기질효응정도불동,기중개별농약재기질중수도보호。본방법피면료보류시간표이、검측결과가양성화봉형타미적문제,결과표명,측정4충유궤린농약잔류량적선성범위균위0.1-0.5mg/L,상관계수위0.9974-0.9989,검출한위0.001-0.009mg/L,3개수평적가표회수솔위80.20%-92.40%,상대표준편차위0.70%-5.47%。
A method to determine multi-residue of methamidophos, phoyate, chlorpyrifos and parathion-methyl in corn protein powder by gas chromatography was discussed in this paper. The residues of organ-phosphorous pesticides in corn protein powder were extracted by ethyl acetate, and the extracts, cleaned up using neutral aluminae and activated carbon. Four types of the target were separated on the DB-1capillary column and detected by FPD detector. Using negative blank sample matrix configuration standard curve, matrix effect degree of pesticides for corn protein powder was different. Few pesticides were protected in the matrix, and the drift of retention time, false positive results and the peak tailing, avoided. The internal method of matrix-matched calibration standard was used for quantification. Satisfactory results were obtained. The linearity was good in the range of 0.1 and 0.5 mg/L with the regression coefficient from 0.9974 to 0.9989. Detection limit ranged from 0.001mg/L to 0.009mg/L, average recoveries of the organ-phosphorous pesticides spiked at 0.1, 0.3 and 0.5 mg/kg were between 80.20 and 92.40%with relative standard deviations of less than 0.70%.