Rapid Determination of Five Alkaloids in Catering Crayfish by QuEChERS-UPLC-MS/MS

YU Ling; SONG Lihua

doi:10.13386/j.issn1002-0306.2022030219

Volume 44 Issue 2

Jan. 2023

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Science and Technology of Food Industry > 2023 > 44(2): 324-331. > DOI: 10.13386/j.issn1002-0306.2022030219

YU Ling, SONG Lihua. Rapid Determination of Five Alkaloids in Catering Crayfish by QuEChERS-UPLC-MS/MS[J]. Science and Technology of Food Industry, 2023, 44(2): 324−331. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2022030219.

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Rapid Determination of Five Alkaloids in Catering Crayfish by QuEChERS-UPLC-MS/MS

YU Ling^{1, 2,},
SONG Lihua^1, ,

1.
School of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai 200240, China
2.
Shanghai Institute for Food and Drug Control, Shanghai 201203, China

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Received Date: March 17, 2022
Available Online: November 20, 2022

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Abstract

Abstract

In this study, a method for the determination of morphine, codeine, nacodine, papaverine and tibain residues in catering crayfish by ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was established. After preparation of crush and mixture, the samples were stirred and dispersed with 0.1 mol/L hydrochloric acid solution and ultrasonic treated for 30 min, then extracted with acetonitrile and QuEChERS powder (6 g anhydrous magnesium sulfate and 1.5 g anhydrous sodium acetate). After centrifugation, the supernatant was pipetted for analysis. The chromatographic separation conditions were as follows: Stationary phase was used ACQUITY UPLCTM BEH HILIC chromatographic column (1.7 μm, 2.1×100 mm). The mobile phase of gradient elution was composed of acetonitrile and 10 mmol/L ammonium formate containing 0.1% formic acid, respectively. The target compounds were analyzed and quantified via electrospray ionization (ESI⁺) mode ionization and multiple reaction monitoring (MRM), and 9 kinds of commercial crayfish were selected as samples for inspection. The results showed that the linear range of internal standard method for quantitative analysis of morphine and codeine was 5~250 ng/mL, and that of external standard method for quantitative analysis of papaverine, nacodine and tibain was 1~50 ng/mL. Within the linear range, the correlation coefficient between peak area and injection concentration (ng/mL) was greater than 0.995. The detection limits and the limits of quantitation of five alkaloids were 0.6~3.7 μg/kg and 2.0~12.4 μg/kg, respectively. The averaged recoveries (n=6) were 80％~110％ and the relative standard deviations (RSDs) were below 10%, and the papaverine and other 5 components were detected in 9 commercial samples. The method was suitable for the qualitative and quantitative analysis of five alkaloids, and was fast, simple, and sensitive.
- ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS),
- QuEChERS,
- alkaloid,
- crayfish

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