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中国精品科技期刊2020
俞灵,宋立华. QuEChERS-UPLC-MS/MS检测餐饮小龙虾中5种生物碱[J]. 食品工业科技,2023,44(2):324−331. doi: 10.13386/j.issn1002-0306.2022030219.
引用本文: 俞灵,宋立华. QuEChERS-UPLC-MS/MS检测餐饮小龙虾中5种生物碱[J]. 食品工业科技,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.
Citation: 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.

QuEChERS-UPLC-MS/MS检测餐饮小龙虾中5种生物碱

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

  • 摘要: 针对市售餐饮小龙虾,利用QuEChERS方法进行前处理,建立超高效液相色谱-串联质谱(UPLC-MS/MS)联用法检测小龙虾中吗啡、可待因、那可丁、罂粟碱、蒂巴因5种生物碱的分析方法。样品经粉碎搅匀制备后用0.1 mol/L盐酸溶液涡旋分散并超声处理30 min,然后利用乙腈及QuEChERS粉末(6 g无水硫酸镁与1.5 g无水醋酸钠)提取,离心后吸取上清溶液进样分析。色谱分离条件为:固定相采用ACQUITY UPLCTM BEH HILIC色谱柱(1.7 μm,2.1×100 mm),流动相采用分别含0.1%甲酸的乙腈和0.1%甲酸的10 mmol/L甲酸铵溶液进行梯度洗脱,经电喷雾正离子(ESI+)模式电离及多反应监测(MRM)分析和定量测定目标化合物,并选用9种市售小龙虾作为试样进行检验。结果表明,内标法定量分析吗啡、可待因的线性浓度范围为5~250 ng/mL,外标法定量分析罂粟碱、那可丁、蒂巴因的线性浓度范围为1~50 ng/mL,在线性范围内峰面积与进样浓度(ng/mL)间的相关系数均大于0.995。5种生物碱的检出限为0.6~3.7 μg/kg,定量限为2.0~12.4 μg/kg,平均加标回收率(n=6)为80%~110%之间,相对标准偏差小于10%,9种市售样品未检出罂粟碱等 5 种组分。该方法操作快速简单、灵敏度高,适用于小龙虾中5种生物碱的定性与定量分析。

     

    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.

     

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