Determination of 23 Organophosphorus Pesticide Residues in Lentinus edodes by High Performance Liquid Chromatography-Tandem Mass Spectrometry

doi:10.7506/spkx1002-6630-201404033

Abstract

Abstract:

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) method was established
for the determination of 23 organophosphorus pesticide residues in Lentinus edodes. Samples were extracted with acetonitrile
and separated by salting out method, and then the supernatants were purified using dispersive solid-phase extraction (C18 and
primary-secondary amine powder) prior to HPLC-MS-MS analysis. The analytes were identified in positive electrospray
ionization and multiple reaction-monitoring modes. The matrix-matched external standard calibration curves were used
for quantitative analysis. Under the optimal conditions, the limit of quantitation of the method was 0.01 mg/kg. The
recoveries of 23 organophosphorus pesticides in spiked real samples were 70.2%–105.0% with relative standard deviation
of 3.5%–13.0%. The method presented is sensitive, accurate and fast and can meet the requirements for the determination of
organophosphorus pesticide residues in Lentinus edodes.

Key words: high performance liquid chromatography-tandem mass spectrometry, organophosphorus pesticide, residues, Lentinus edodes

CLC Number:

TS207.3

LIANG Da-qing, SU Ken-ming, ZHANG Ju-mei, GUO Wei-peng. Determination of 23 Organophosphorus Pesticide Residues in Lentinus edodes by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2014, 35(4): 159-162.

References

[1] 张书香，谢建春，斳林溪，等. 同时蒸馏萃取/气-质联用分析黑龙江香菇香味成分[J]. 精细化工，2010,27（5）：456-462.

[2] 陶名熏. 香菇的药效和食品开发[J]. 食品科学，1986,7（1）：11-13.

[3] 王会锋，冯书惠，贾斌. 香菇中40种农药残留量的气相色谱法测定[J]. 食品科学，2010,31（20）：335-341.

[4] 李艳芳，叶瑜霏，罗华建，等. 气相色谱-火焰光度法测定黑木耳中16种有机磷农药残留[J]. 广东农业科学，2011,（18）：138-139.

[5] 潘守奇，孙军，董静，等. 气相色谱法同时测定蔬菜中24种有机磷农药残留[J]. 分析试验室，2010，29（1）：115-118.

[6] NY/T 761-2008 蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].

[7] GB/T 5009.20-2003 食品中有机磷农药残留量的测定[S].

[8] GB/T 5009.103-2003 植物性食品中甲胺磷和乙酰甲胺磷农药残留量的测定[S].

[9] GB/T 5009.109-2003 柑桔中水胺硫磷残留量的测定[S].

[10] GB/T 5009.207-2008 糙米中50种有机磷农药残留量的测定[S].

[11] ARAZ B , MOHAMMAD R G , PARVIZ N , et al. Sample preparation method for the analysis of some organophosphorus pesticides residues in tomato by ultrasound-assisted solvent extraction followed by dispersive liquid–liquid microextraction[J],Food Chemistry, 2011, 126(4): 1840-1844.

[12] FEMANDEZ M ,PADRON C , MARCONI L, et al. Determination of organophosphorus pesticides in honeybees after solid-phase microextraction[J], Journal of Chromatography A, 2001,922(1-2):257-265.

[13] 白冰，董茂锋，邢增涛，等. 气相色谱-质谱法检测双孢蘑菇和香菇中的67种农药残留[J]. 食用菌学报，2011,18（1）：63-69.

[14] 于桂兰，李万红，液液萃取-气相色谱质谱法测定饮用水中19种有机磷农药[J]. 中国卫生检验杂志，2012, 22（6）：1283-1285.

[15] SU Rui , XU Xu, WANG Xinghua , et al. Determination of organophosphorus pesticides in peanut oil by dispersive solid phase extraction gas chromatography–mass spectrometry[J],Journal of Chromatography B, 2011,879(30):3423-3428.

[16] 刘庆斌，张睿，王海涛，等. 高效液相色谱串联质谱法对栀子中11种有机磷农药残留的检测[J]. 分析测试学报，2010,29（1）：73-76.

[17] GB/T 20769-2008 水果和蔬菜中450种农药及相关化学品残留量的测定液相色谱-串联质谱法[S].

[18] 黄和勇，陈其煌，高效液相色谱-串联质谱法测定韭菜中12种有机磷农药残留效果研究[J]. 现代农业科技，2012,（18）：295-298.

[19] HUANG Fang , SHEN Yu-Dong , LEI Hong-Tao, et al. Monitoring of organophosphorus pesticides in vegetables using monoclonal antibody-based direct competitive ELISA followed by HPLC–MS/MS[J], Food Chemistry, 2012，131( 4): 1569-1576.

[20] BENNO A, RUUD C, ROB J , et al. Determination of polar organophosphorus pesticides in aqueous samples by direct injection using liquid chromatography–tandem mass spectrometry[J], Journal of Chromatography A, 2001，918(1): 67-78.