Rapid Determination of Residues of Fenpropathrin Enantiomers in Fruit Puree of Infant Dietary Supplement by Ultra-High Performance Convergence Chromatography
摘 要
在5 g婴幼儿辅食果泥样品中加入乙酸乙酯20 mL和氯化钠3.0 g,涡旋2 min,离心5 min,用20 mL乙酸乙酯重复提取一次,合并两次上清液,于40℃减压浓缩至近干,加入5 mL甲醇溶解残渣。所得溶液过活化好的C18固相萃取柱,收集全部流出液,于40℃氮吹至近干,加入1 mL正庚烷,涡旋1 min溶解残渣,过0.22 μm有机相滤膜,滤液用超高效合相色谱法(UPC2)分析。以Acquity Trefoil AMY1色谱柱为固定相,以不同体积比的含0.5%(体积分数)氨水的甲醇溶液和超临界二氧化碳的混合溶液为流动相进行梯度洗脱,在230 nm波长下检测(-)-甲氰菊酯和(+)-甲氰菊酯,外标法定量。结果显示,甲氰菊酯对映体的质量浓度在1.0~20.0 mg·L-1内和对应的峰面积呈线性关系,测定下限(10S/N)均为0.2 mg·kg-1。对阴性果泥样品进行3个浓度水平的加标回收试验,两种目标物的回收率为81.4%~106%,测定值的相对标准偏差(n=6)为4.1%~7.2%。方法用于20份果泥样品的分析,仅在1份梨泥样品中检出(-)-甲氰菊酯(0.25 mg·kg-1)和(+)-甲氰菊酯(0.22 mg·kg-1)。
Abstract
Ethyl acetate (20 mL) and 3.0 g of sodium chloride were added into 5 g of fruit puree of infant dietary supplement sample. The mixture was vortexed for 1 min, and centrifuged for 5 min. The extraction was repeated once with 20 mL of ethyl acetate. The two supernatants were combined and evaporated to near dryness under vacuum at 40℃. The residue was dissolved in 5 mL of methanol. The solution was passed through the activated C18 solid phase extraction column, and the entire effluent was collected, and dried to near dryness by nitrogen at 40℃. Then 1 mL of heptane was added, and vortex process was made for 1 min to dissolve the residue. The solution obtained was filtered through a 0.22 μm organic phase filter membrane, and the filtrate was analyzed by UPC2. Acquity Trefoil AMY1 column was used as the stationary phase. Mixed solutions composed of methanol solution containing 0.5% (φ) ammonia and supercritical carbon dioxide at different volume ratios were used as the mobile phase for gradient elution. (-)-Fenpropathrin and (+)-fenpropathrin were determined by external standard method at detection wavelength of 230 nm. It was shown that linear relationships between values of the mass concentration and peak area of the fenpropathrin enantiomers were kept in the range of 1.0-20.0 mg·L-1, with lower limits of determination (10S/N) of 0.2 mg·kg-1. The spiked recovery test was made at three concentration levels on the negative fruit puree samples, giving recoveries of the 2 targets in the range of 81.4%-106%, and RSDs (n=6) of the determined values in the range of of 4.1%-7.2%. The proposed method was used for the analysis of 20 fruit puree samples, and (-)-fenpropathrin (0.25 mg·kg-1) and (+)-fenpropathrin (0.22 mg·kg-1) were detected in one pear puree sample.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202311008
所属栏目 工作简报
基金项目 科技部国家重点研发计划政府间合作项目(2019YFE0103900)
收稿日期 2022/3/27
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备注张文华,高级工程师,博士,研究方向为食品中药物残留分析,zwh@zaiq.org.cn
引用该论文: ZHANG Wenhua,XIE Wen,HOU Jianbo,ZHANG Yunjie,XU Hui,LOU Chengjie,SONG Wei,HAN Fang. Rapid Determination of Residues of Fenpropathrin Enantiomers in Fruit Puree of Infant Dietary Supplement by Ultra-High Performance Convergence Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(11): 1290~1296
张文华,谢文,侯建波,张蕴杰,徐绘,楼成杰,宋伟,韩芳. 超高效合相色谱法快速测定婴幼儿辅食果泥中甲氰菊酯对映体的残留量[J]. 理化检验-化学分册, 2023, 59(11): 1290~1296
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【2】朱美娜,李朝阳,李巧玲,等.土壤中甲氰菊酯对映体选择性降解的研究[J].江苏农业科学, 2011,39(6):481-483.
【3】高如瑜,祝凌燕,陈志远.手性菊酯类农药甲氰菊酯、氟胺氰菊酯光学异构体在HPLC上的分离[J].农药, 1998,37(9):22-24.
【4】国家卫生健康委员会,农业农村部,国家市场监督管理总局.食品安全国家标准食品中农药最大残留限量:GB 2763-2021[S].北京:中国标准出版社, 2021.
【5】WAKABAYASHI M, WAKABAYASHI H, RIEGEL A D, et al. Analytical and sensory characterization of the stereoisomers of 3-mercaptocycloalkanones and 3-mercaptocycloalkanols[J]. Journal of Agricultural and Food Chemistry, 2020,68(27):7184-7193.
【6】BALINT A, CÂRJE A G, MUNTEAN D L, et al. Research article. the influence of some parameters on chiral separation of ibuprofen by high-performance liquid chromatography and capillary electrophoresis[J]. Acta Medica Marisiensis, 2017,63(1):36-40.
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【8】DUELL A K, KERBER P J, LUO W T, et al. Determination of (R)-(+)- and (S)-(-)-nicotine chirality in puff bar E-liquids by 1H NMR spectroscopy, polarimetry, and gas chromatography-mass spectrometry[J]. Chemical Research in Toxicology, 2021,34(7):1718-1720.
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【10】KARAKKAKAL A K, KARATT T K, PHILIP M, et al. Separation and determination of the enantiomeric levamisole and dexamisole in equine plasma samples using chiral polysaccharide column/LC-MS/MS[J]. Current Analytical Chemistry, 2020,16(6):761-767.
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【14】SUTHAR S K, RAUSCHER A Á, WINTERNITZ M, et al. Chiral HPLC separation of enantiomeric blebbistatin derivatives and racemization analysis in vertebrate tissues[J]. Journal of Pharmaceutical and Biomedical Analysis, 2021,204:114246.
【15】JING X, HUANG X, WANG H H, et al. Popping candy-assisted dispersive liquid-liquid microextraction for enantioselective determination of prothioconazole and its chiral metabolite in water, beer, Baijiu, and vinegar samples by HPLC[J]. Food Chemistry, 2021,348:129-147.
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【18】ZHANG W H, XIE W, HOU J B, et al. Analytical research on the separation and residue of chiral pesticide triadimenol in fruit and vegetable puree[J]. Journal of Separation Science, 2021,44(18):3516-3523.
【19】张文华,谢文,侯建波,等.基于超高效合相色谱技术的保健食品中肉碱对映体拆分和测定方法研究[J].分析测试学报, 2021,40(12):1713-1719.
【20】张文华,谢文,侯建波,等.超高效合相色谱法拆分和测定婴幼儿配方乳粉中肉碱对映体[J].理化检验-化学分册, 2021,57(11):970-976.
【21】张文华,洪灯,雷美康,等.超高效合相色谱法拆分和测定克伦特罗对映体[J].色谱, 2021,39(12):1347-1354.
【22】张文华,侯建波,荣杰峰,等.超高效合相色谱法对克伦特罗对映体的拆分及其在猪尿中的残留分析[J].分析测试学报, 2021,40(12):1758-1764.
【23】李敏青,安文佳,李菊,等.固相萃取/气相色谱法测定禽蛋中19种农药残留[J].分析测试学报, 2020,39(4):520-525.
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