高效液相色谱法测定番茄中腐霉利和异菌脲的残留量
目的建立固相萃取-高效液相色谱法测定番茄中腐霉利和异菌脲的残留量。方法番茄样品用乙腈超声提取,加入氯化钠进行盐析脱水,提取液过Florisil柱净化,用正己烷/丙酮(90:10,V:V)淋洗液洗脱,洗脱液氮吹近干,甲醇定容后经ZORBAX Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱进行分离,以乙腈/水(60:40,V:V)为流动相,流速为1.0 m L/min,采用二极管阵列检测器检测,检测波长为208 nm。结果在0.055.0 mg/L浓度范围内,腐霉利和异菌脲的质量浓度与其峰面积呈良好的线性关系(r2〉0.999),方法检出限均为0.025 mg/kg,在...
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Published in | 食品安全质量检测学报 Vol. 8; no. 2; pp. 486 - 490 |
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Main Author | |
Format | Journal Article |
Language | Chinese |
Published |
平湖市食品药品检测中心,平湖,314200
2017
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Subjects | |
Online Access | Get full text |
ISSN | 2095-0381 |
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Summary: | 目的建立固相萃取-高效液相色谱法测定番茄中腐霉利和异菌脲的残留量。方法番茄样品用乙腈超声提取,加入氯化钠进行盐析脱水,提取液过Florisil柱净化,用正己烷/丙酮(90:10,V:V)淋洗液洗脱,洗脱液氮吹近干,甲醇定容后经ZORBAX Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱进行分离,以乙腈/水(60:40,V:V)为流动相,流速为1.0 m L/min,采用二极管阵列检测器检测,检测波长为208 nm。结果在0.055.0 mg/L浓度范围内,腐霉利和异菌脲的质量浓度与其峰面积呈良好的线性关系(r2〉0.999),方法检出限均为0.025 mg/kg,在0.05、0.5和1.0 mg/kg 3个不同加标水平上,腐霉利和异菌脲的加标回收率为90.6%102.4%,精密度为3.72%6.55%。结论该方法操作简单、准确,可应用于番茄中腐霉利和异菌脲的检测。 |
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Bibliography: | Objective To establish a method for determination of procymidone and iprodione residues in tomato by solid phase extraction-high performance liquid chromatography(SPE-HPLC). Methods After ultrasonic extraction with acetonitrile, the tomato extracts were added sodium chloride to salt out, purified by Florisil column, eluted by the purified solution with n-hexane/acetone(90:10, V:V), blown by nitrogen evaporator until it was almost dry and diluted with methyl alcohol to a constant volume. Then it was separated by a ZORBAX Eclipse XDB-C18column(250 mm×4.6 mm, 5 μm) using acetonitrile/water(60:40, V:V) as mobile phase at the flow rate of 1.0 m L/min, and detected by diode array detector(DAD) at 208 nm. Results Procymidone and iprodione had good linear relationships between mass concentration and peak area(r2 〉0.999) in the range of 0.055.0 mg/L. The detection limits of two pesticides were both 0.025 mg/kg. The recoveries spiked at 3 levels of 0.05, 0.5 and 1.0 mg/kg were 90.6%102.4% with RSD of 3.72%6.55%. Conclu |
ISSN: | 2095-0381 |