加速溶剂萃取结合气相色谱-三重四极杆质谱测定枸杞中有机磷农药多残留
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摘要
建立了加速溶剂萃取与气相色谱-三重四极杆质谱联用(GC-MS/MS)法对枸杞中20种有机磷农药残留进行测定。样品经酸化乙腈-二氯甲烷(体积比4∶1)提取,Cleanert TPH固相萃取柱净化,旋转蒸发浓缩后氮吹至干,采用GC-MS/MS检测,并对萃取溶剂、温度、冲洗体积等实验条件进行了优化。结果表明,20种药物在1～500μg/kg范围内线性良好,相关系数(r~2)为0.999 0～0.999 8;在20、40、100μg/kg 3个加标水平下的回收率为70.0%～82.9%,相对标准偏差(RSD,n=5)为0.6%～8.5%,定量下限为1～15μg/kg。该方法样品前处理简单、定量准确,适用于枸杞中有机磷农药残留的检测。
A gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS) with accelerated solvent extraction was developed for the determination of 20 organophosphorus pesticides residues in Chinese wolfberry.The samples were first extracted with acidified acetonitrile-dichloromethane(4 ∶1,by volume),then purified on a Cleanert TPH solid phase extraction column,next concentrated by rotary evaporation and dried with nitrogen,and finally analyzed by GC-MS/MS.The experimental conditions such as extraction solvent,temperature and rinse volume were optimized.Results showed that the calibration curves for 20 pesticides were linear in the range of 1-500 μg/kg with their correlation coefficients(r~2) of 0.999 0-0.999 8.The spiked recoveries at three levels of 20,40 and 100 μg/kg were in the range of 70.0%-82.9% with the relative standard deviations(RSDs,n=5) of 0.6%-8.5%.The limits of quantitation of the method ranged from 1.0 μg/kg to 15.0 μg/kg.The method is simple and accurate,and is suitable for the determination of organophosphorus pesticide residues in Chinese wolfberry.
A gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS) with accelerated solvent extraction was developed for the determination of 20 organophosphorus pesticides residues in Chinese wolfberry.The samples were first extracted with acidified acetonitrile-dichloromethane(4 ∶1,by volume),then purified on a Cleanert TPH solid phase extraction column,next concentrated by rotary evaporation and dried with nitrogen,and finally analyzed by GC-MS/MS.The experimental conditions such as extraction solvent,temperature and rinse volume were optimized.Results showed that the calibration curves for 20 pesticides were linear in the range of 1-500 μg/kg with their correlation coefficients(r~2) of 0.999 0-0.999 8.The spiked recoveries at three levels of 20,40 and 100 μg/kg were in the range of 70.0%-82.9% with the relative standard deviations(RSDs,n=5) of 0.6%-8.5%.The limits of quantitation of the method ranged from 1.0 μg/kg to 15.0 μg/kg.The method is simple and accurate,and is suitable for the determination of organophosphorus pesticide residues in Chinese wolfberry.
引文
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[2] Bondia-Pons I,Savolainen O,T?rr?nen R,Martinez J A,Poutanen K,Hanhineva K.Food Res.Int.,2014,63:132-138.
[3] Cheng D,Kong H.Molecules,2011,16(3):2542-2550.
[4] Amagase H,Farnsworth N R.Food Res.Int.,2011,44(7):1702-1717.
[5] Bi M C.The Effect and Mechanism of Zeaxanthin Inducesapoptosis and Inhibit Cell Migration,Invasion in Human Uvealmelanoma Cells.Changchun:Jilin University(毕明超.玉米黄素对人葡萄膜黑色素瘤细胞凋亡和迁移的作用及其机制研究.长春:吉林大学),2016.
[6] Jeszka-Skowron M,Zgo?a-Grze:228-236.
[7] Fu Y,Yang T,Zhao J,Zhang L,Chen R X,Wu Y L.Food Chem.,2017,218:192-198.
[8] Ren Y P,Hu Z Q.J.Ningxia Agr.College(任月萍,胡忠庆.宁夏农学院学报),2004,(3):88-91.
[9] Liu D J.Study on Determination of 100 Pesticide Residues in Fructus Lunch by Gas Choramatogramy-Mass and Three Aromatic Tradition Chinese Medicine Quality Research.Beijing:Chinese Union Medical University(刘东静.枸杞药材中100种农药多残留GC-MSn测定方法研究及三种芳香类药材质量研究.北京:中国协和医科大学),2010.
[10] Zhou W N.Agr.Inf.Chin.(周维娜.中国农业信息),2013,(15):164.
[11] Lu L L.Study on Analysis of Pesticides Multiresidues in Ephedrae and Medlar.Shihezi:Shihezi University(鲁立良.麻黄和枸杞中农药多残留分析方法研究.石河子:石河子大学),2007.
[12] Wang J,Cao S R,Zhang L,Xu F,Wang G M,Li X L.J.Instrum.Anal.(王均,曹淑瑞,张雷,徐芬,王国民,李贤良.分析测试学报),2013,32(11):1309-1315.
[13] Cao D J.J.Chifeng Univ.(曹殿洁.赤峰学院学报),2013,29(11):6-7.
[14] Zheng Z T,Gong Y,Sun F S,Cui K,Pu X Y,Li F G.Pesticides(郑尊涛,龚勇,孙丰收,崔凯,朴秀英,李富根.农药),2018,57(11):826-828,839.
[15] Liang Y X,Wang X J,Jiang R,Wu Y,Niu Y.Shandong Forestry Sci.Technol.(梁月香,王晓菁,姜瑞,吴燕,牛艳.山东林业科技),2011,41(6):1-4.
[16] Li L,Jiang S R,Pan C P,Zhou Z Q,Qian C F,Liu F M.J.Pestic.(李莉,江树人,潘灿平,周志强,钱传范,刘丰茂.农药学学报),2006,(4):371-374.
[17] Li L Q.Analy of Pesticide Multiresidues in Chinese Medicianal Herbs.Hangzhou:Zhejiang University(李丽青.中药材中农药多残留分析方法研究.杭州:浙江大学),2005.
[18] Zhang T T.Determination of Multi-pesticide Residues in Dried Fruits and Nuts by UPLC-MS/MS.Urumqi:Xinjiang University(张婷亭.新疆干坚果品中农药多残留的前处理和UPLC-MS/MS分析方法的研究.乌鲁木齐:新疆大学),2016.
[19] National Standards of the Pecple's Republic of China.GB 23200.10—2016.Food Safety National standard:Determination of 488 Pesticides and Related Chemicals Residues in Mulberry Branch,Honeysuckle,Wolfberry and Lotus Leaf by Gas Chromatography-Mass Spectrometry(中华人民共和国国家标准.GB 23200.10—2016.食品安全国家标准:桑枝、金银花、枸杞子和荷叶中488种农药及相关化学品残留量的测定气相色谱-质谱法).
[20] Yang D F,Liu T F,Fan J,Sun X L,Lu H Q,Qian H.Env.Sustainable Dev.(杨代凤,刘腾飞,范君,孙灵湘,陆皓茜,钱辉.环境与可持续发展),2018,(6):219-221.
[21] Zhang B L,Pang G F,Feng C,Li J X,Wu X Q,Hu X Y,Fan C L.J.Instrum.Anal.(张博伦,庞国芳,冯春,李建勋,吴兴强,胡雪艳,范春林.分析测试学报),2018,37(6):653-659.