Determination of 11 kinds of pesticide residues in liquid milk by dispersive solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

Authors

HUANG Mangu, Guangzhou Inspection Testing and Certification Group Co., Ltd., Guangzhou, Guangdong 511447, China;National Quality Inspection and Testing Center for Processed Foods 〔Guangdong〕, Guangzhou, Guangdong 511447, ChinaFollow
LUO Yonghao, Guangzhou Inspection Testing and Certification Group Co., Ltd., Guangzhou, Guangdong 511447, China;National Quality Inspection and Testing Center for Processed Foods 〔Guangdong〕, Guangzhou, Guangdong 511447, China
YAN Wanying, Guangzhou Inspection Testing and Certification Group Co., Ltd., Guangzhou, Guangdong 511447, China;National Quality Inspection and Testing Center for Processed Foods 〔Guangdong〕, Guangzhou, Guangdong 511447, China
XU Lizhu, Guangzhou Inspection Testing and Certification Group Co., Ltd., Guangzhou, Guangdong 511447, China;National Quality Inspection and Testing Center for Processed Foods 〔Guangdong〕, Guangzhou, Guangdong 511447, China

Abstract

Objective： This study aimed to evaluate the safety of pesticide residues in liquid milk. Methods： A method for simultaneous determination of 11 kinds of pesticide residues by ultra-high-performance liquid chromatography-tandem mass spectrometry was established. The samples were extracted by acetonitrile, purified by C₁₈ and PSA solid phase extractants, separated on a column Xbridge BEH C₁₈ (100 mm×2.1 mm, 1.7 μm), determined in multi-reaction monitoring mode, and optimized for pre-treatment parameters using response surface method. Results： The optimal conditions for pretreatment were 10 mL acetonitrile, 50 mg C₁₈ and 30 mg PSA. The linear relationships of 11 kinds of pesticides were good in the concentration range of 1.0~100.0 μg/L, and the correlation coefficients (R²) were all > 0.999. With addition of 10, 20, 100 μg/kg, the average recoveries were 82.7%～102.0%, the relative standard deviations were 2.89% to 8.87%, and the limits of detection (LOD) and limits of quantitation (LOQ) were 2.0～3.0 μg/kg and 5.0～10.0 μg/kg, respectively. Conclusion： The method is simple, convenient, rapid, high recovery rate and high reproducibility, which could accurately determine 11 kinds of pesticide residues in liquid milk.

Publication Date

1-30-2024

First Page

48

Last Page

54,87

DOI

10.13652/j.spjx.1003.5788.2022.81068

Recommended Citation

Mangu, HUANG; Yonghao, LUO; Wanying, YAN; and Lizhu, XU (2024) "Determination of 11 kinds of pesticide residues in liquid milk by dispersive solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry," Food and Machinery: Vol. 39: Iss. 12, Article 8.
DOI: 10.13652/j.spjx.1003.5788.2022.81068
Available at: https://www.ifoodmm.cn/journal/vol39/iss12/8

References

[1] 崔家瑞. 我国乳制品业发展的现状、问题及措施[J]. 食品安全导刊, 2018（15）: 47-48. CUI J R. Current situation, problems and measures of dairy industry development in China[J]. China Food Safety, 2018（15）: 47-48.
[2] HAHNE J, ISELE D, BERNING J, et al. The contribution of fast growing psychrotrophic microorganisms on biodiversity of refrigerated raw cow's milk with high bacterial counts and their food spoilage potential[J]. Food Microbiol, 2018, 79: 11-19.
[3] JIA W, SHI L, CHU X. Dissociation mechanisms-based UHPLC Q-Orbitrap strategy for screening of cephalosporins and metabolites in shrimp[J]. Food Chem, 2018, 250（1）: 30-36.
[4] GAO D, CHEN S H, ZHANG Q, et al. Simultaneous determination of 35 organophosphorus pesticide residues in wheat flour by gas chromatography[J]. J Food Safe Quality, 2015（4）: 1 116-1 121.
[5] 戴洋洋, 闫磊, 王春天, 等. 气相色谱电子捕获检测器测定生鲜乳中有机氯农药残留[J]. 中国乳业, 2018（12）: 63-65. DAI Y Y, YAN L, WANG C T, et al. Determination of organochlorine pesticide residues in fresh milk by gas chromatography with electron capture detector[J]. China Dairy, 2018（12）: 63-65.
[6] HARSHIT D, CHARMY K, NRUPESH P. Organophosphorus pesticides determination by novel HPLC and spectrophotometric method[J]. Food Chem, 2017, 230: 448-453.
[7] 徐潇颖, 朱炳祺, 刘柱, 等. 气相色谱—质谱法测定含乳饮料中5种农药残留[J]. 分析科学学报, 2019, 35（4）: 525-528. XU X Y, ZHU B Q, LIU Z, et al. Simultaneous determination of five pesticide residues in milk beverages by gas chromatography-mass spectrometry[J]. J Analyt Sci, 2019, 35（4）: 525-528.
[8] 杨会会, 娄芳慧, 韩二芳, 等. QuEChERS-气相色谱—质谱法同时测定香蕉酸奶中5种拟除虫菊酯类农药残留[J]. 中国乳品工业, 2018, 46（10）: 36-39. YANG H H, LOU F H, HAN E F, et al. Determination of 5 pyrethroid pesticides in banana yogurt by QuEChERS-gas chromatography-mass spectrometry[J]. China Dairy Industry, 2018, 46（10）: 36-39.
[9] LAURA M M, MICHAEL J T. Use of a deactivated PTV injector liner and GC-MS/MS for the quantitative determination of multiple pesticide residues in fruit and vegetables[J]. MethodsX, 2020, 8: 101180.
[10] 谢瑞龙, 梁建英. 气相色谱—串联质谱法测定豆乳中12种有机磷及氨基甲酸酯类农药残留[J]. 乳业科学与技术, 2021, 44（5）: 27-31. XIE R L, LIANG J Y. Determination of 12 organophosphorus and carbamate pesticide residues in soy milk by gas chromatography-tandem mass spectrometry[J]. J Dairy Sci Technol, 2021, 44（5）: 27-31.
[11] ANTONIO J N G, ROBERTO R G, ANTONIA G F. Determination of multi-class pesticide residue in dietary supplements from grape seed extracts by ultra-high-performance liquid chromatography coupled to triple quadrupole mass spectrometry[J]. Food Addit Contam A, 2014, 31（9）: 1 550-1 561.
[12] 黄小波, 刘维平. 基于QuEChERS的UHPLC-MS/MS同时检测鸡蛋中19种农药残留量[J]. 食品与机械, 2021, 37（10）: 56-60. HUANG X B, LIU W P. Simultaneous determination of 19 kinds of pesticide residues in eggs by UHPLC-MS/MS based on QuEChERS[J]. Food & Machinery, 2021, 37（10）: 56-60.
[13] 陈锦杭, 冯城婷, 林秋凤, 等. QuEChERS-固相萃取—气相色谱/四极杆飞行时间质谱法快速测定牛奶中的11种有机磷[J]. 中国乳品工业, 2021, 49（1）: 51-54. CHEN J H, FENG C T, LIN Q F, et al. Rapid determination of eleven organic phosphorus in milk by QuEChERS-SPE coupled with gas chromatography-quadrupole time of flight mass spectrometry[J]. China Dairy Industry, 2021, 49（1）: 51-54.
[14] 贾玮, 张荣, 陈雪峰, 等. 分散固相萃取—超高效液相色谱—四极杆—静电场轨道离子阱质谱测定巴氏杀菌乳中农药残留[J]. 陕西科技大学学报, 2019, 37（3）: 64-69. JIA W, ZHANG R, CHEN X F, et al. Dispersive solid phase extraction coupled with ultra performance liquid chromatography-quadrupole-orbitrap mass spectrometry for determination of pesticide residues in pasteurized milk[J]. Journal of Shaanxi University of Science, 2019, 37（3）: 64-69.
[15] 韩镌竹, 田晓玲, 李香珍, 等. 超高效液相色谱—串联质谱法测定生鲜乳中6种农药的残留[J]. 中国畜牧兽医, 2013, 40（S1）: 62-67. HAN J Z, TIAN X L, LI X Z, et al. Determination on 6 kinds of pesticide residues in the raw milk by ultra performance liquid chromatography-tandem mass spectrometry[J]. China Animal Husbandry and Veterinary Medicine, 2013, 40（S1）: 62-67.
[16] 田宏哲, 赵瑛博, 周艳明. 高效液相色谱—质谱法测定牛奶中6种氨基甲酸酯农药残留[J]. 食品科学, 2011, 32（2）: 187-190. TIAN H Z, ZHAO Y B, ZHOU Y M. Simultaneous determination of six carbamate pesticide residues in milk by HPLC-ESI-MS/MS[J]. Food Sci, 2011, 32（2）: 187-190.
[17] 区硕俊, 岑建斌, 梁俊发, 等. 酰胺化衍生—高效液相色谱—四极杆—高分辨飞行时间质谱法测定食品接触塑料材料中7种烷基胺[J]. 分析化学, 2020, 48（3）: 413-422. OU S J, CEN J B, LIANG J F, et al. Determination of seven kinds of alkylamines in food contact plastic materials by amidation coupled with high performance liquid chromatography-quadrupole time-of-flight mass spectrometer[J]. Chinese J Anal Chem, 2020, 48（3）: 413-422.
[18] 陈建彪, 董丽娜, 刘娇, 等. QuEChERS在食品中真菌毒素检测的研究进展[J]. 食品科学, 2014, 35（11）: 286-291. CHEN J B, DONG L N, LIU J, et al. Advances in application of QuEChERS for mycotoxin analysis in foods[J]. Food Sci, 2014, 35（11）: 286-291.