Determination of jingangmycin and propiconazole in Atractylodes macrocephala by solid phase extraction/ultrahigh performance liquid chromatography-tandem mass spectrometry

doi:10.3969/j.issn.1004-1524.2022.12.18

Acta Agriculturae Zhejiangensis ›› 2022, Vol. 34 ›› Issue (12): 2750-2758.DOI: 10.3969/j.issn.1004-1524.2022.12.18

• Quality and Safety of Agricultural Products • Previous Articles Next Articles

Determination of jingangmycin and propiconazole in Atractylodes macrocephala by solid phase extraction/ultrahigh performance liquid chromatography-tandem mass spectrometry

ZHANG Chunrong(), GUO Qian, KONG Liping, WU Yuanyuan, LIN Qin, XU Zhenlan, TANG Tao()

State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-Products/Key Laboratory for Pesticide Residue Detection of Ministry of Agriculture and Rural Affairs/Institute of Agro-Product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China

Received:2021-09-28 Online:2022-12-25 Published:2022-12-26
Contact: TANG Tao

Abstract

Abstract:

A simple and sensitive method was developed for the determination of jingangmycin A and propiconazole in fresh and dry samples of Atractylodes macrocephala by solid phase extraction/ultrahigh performance liquid chromatography-tandem mass spectrometry (SPE/UPLC-MS/MS). The samples were extracted with methanol/water(9∶1, V/V),purified with an Oasis HLB column (for jingangmycin A) and Cleanert AQ C18 column (for propiconazole),and separated on a HSS T3 column,finally analyzed in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI⁺). Under the optimum condition,the calibration curves for the analyte were linear in the range of 0.000 1-0.1 mg·L^-1,with correlation coefficients(R²) not less than 0.999 6. At spiked levels of 0.01,0.5 and 5.0 mg·kg^-1,the recoveries for jingangmycin A in two matrices were in the range of 72.4%-85.8% with relative standard deviations(RSD) of 0.89%-6.20%; At spiked levels of 0.005,0.1 and 1.0 mg·kg^-1,the recoveries for propiconazole in two matrices were in the range of 88.1%-98.9% with relative standard deviations(RSD) of 1.4%-4.8%. The method was simple, reproducible, accurate, precise and the detection limit could meet the requirements of pesticide residue analysis.

Key words: jingangmycin A, propiconazole, Atractylodes macrocephala, ultrahigh performance liquid chromatography-tandem mass spectrometry, residues

CLC Number:

S567.233

ZHANG Chunrong, GUO Qian, KONG Liping, WU Yuanyuan, LIN Qin, XU Zhenlan, TANG Tao. Determination of jingangmycin and propiconazole in Atractylodes macrocephala by solid phase extraction/ultrahigh performance liquid chromatography-tandem mass spectrometry[J]. Acta Agriculturae Zhejiangensis, 2022, 34(12): 2750-2758.

Figures/Tables 8

References 26

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化合物 Compound	母离子 Precursor ion(m/z)	子离子 Product ion(m/z)	驻留时间 Retention time/ms	Q1偏转电压 Q1 bias voltage/V	碰撞能量 Collision energy/eV	Q3偏转电压 Q3 bias voltage/V
井冈霉素Jiangangmycin A	498.10	178.2^*,124.3	100	-24,-25	-26,-40	-21,-27
丙环唑Propiconazole	341.90	159.0^*,69.1	100	-24,-25	-35,-21	-18,-28

化合物 Compound	母离子 Precursor ion(m/z)	子离子 Product ion(m/z)	驻留时间 Retention time/ms	Q1偏转电压 Q1 bias voltage/V	碰撞能量 Collision energy/eV	Q3偏转电压 Q3 bias voltage/V
井冈霉素Jiangangmycin A	498.10	178.2^*,124.3	100	-24,-25	-26,-40	-21,-27
丙环唑Propiconazole	341.90	159.0^*,69.1	100	-24,-25	-35,-21	-18,-28

农药 Pesticide	基质 Matrix	添加浓度 Spiked concentration/(mg·kg^-1)	平均回收率 Average recovery/%	RSD/%
井冈霉素Jiangangmycin A	鲜样Fresh samples	0.01、0.5、5.0	72.4、83.5、85.8	3.0、2.8、2.9
	干样Dry samples	0.01、0.5、5.0	85.5、78.1、79.6	6.2、2.1、0.89
丙环唑Propiconazole	鲜样Fresh samples	0.005、0.1、1.0	90.8、96.9、92.4	3.7、2.9、2.3
	干样Dry samples	0.005、0.1、1.0	98.9、93.3、88.1	4.8、1.4、3.0

农药 Pesticide	基质 Matrix	添加浓度 Spiked concentration/(mg·kg^-1)	平均回收率 Average recovery/%	RSD/%
井冈霉素Jiangangmycin A	鲜样Fresh samples	0.01、0.5、5.0	72.4、83.5、85.8	3.0、2.8、2.9
	干样Dry samples	0.01、0.5、5.0	85.5、78.1、79.6	6.2、2.1、0.89
丙环唑Propiconazole	鲜样Fresh samples	0.005、0.1、1.0	90.8、96.9、92.4	3.7、2.9、2.3
	干样Dry samples	0.005、0.1、1.0	98.9、93.3、88.1	4.8、1.4、3.0

化合物 Compound	时间 Time/d	浙江省Zhejiang Province		湖南省Hunan Province		安徽省Anhui Province		湖北省Hebei Province
化合物 Compound	时间 Time/d	鲜样 Fresh samples	干样 Dry samples	鲜样 Fresh samples	干样 Dry samples	鲜样 Fresh samples	干样 Dry samples	鲜样 Fresh samples	干样 Dry samples
井冈霉素	28	<0.010	<0.010	<0.010	<0.010	<0.010	<0.010	<0.010	<0.010
Jiangangmycin A	35	<0.010	<0.010	<0.010	<0.010	<0.010	<0.010	<0.010	<0.010
丙环唑	28	0.020	0.040	0.012	0.042	0.009 6	0.024	0.046	0.12
Propiconazole	35	0.010	0.036	0.008 3	0.028	<0.005	0.010	0.036	0.098

Determination of jingangmycin and propiconazole in Atractylodes macrocephala by solid phase extraction/ultrahigh performance liquid chromatography-tandem mass spectrometry

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