Rapid screening of illegally added poppy husk in hot pot sauce and soup by thermal desorption electrospray ionization-triple quadruple mass spectrometry

doi:10.3724/SP.J.1123.2020.02002

Abstract

Abstract:

A thermal desorption electrospray ionization-triple quadruple mass spectrometry (TD-ESI-MS/MS) method was developed for the rapid screening of poppy husk in hot pot sauce and soup. The solid surface or liquid sample was directly touched by a simple metal probe. The analytes collected on the probe were desorbed and ionized using a TD-ESI source, after which the analyte ions were detected by MS/MS in multiple reaction monitoring (MRM) mode. The results were compared with those of colloidal gold card rapid detection and verified by high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-MS/MS). The instrument gave the best response with the highest sensitivity under the following conditions: thermal desorption temperature, 260 ℃; injection solvent, 0.1% formic acid aqueous solution containing 10 mmol/L formic ammonium-acetonitrile (1:1, v/v); flow rate, 200 μL/h. The limits of detection (LODs) for papaverine, noscapine, and thebaine in five alkaloids were 2 μg/kg, while those for codeine and morphine were 10 μg/kg in hot pot sauce and 5 μg/kg in soup. The sensitivity of this method was significantly superior to that of the colloidal gold card rapid detection. The method was applied to 50 batches of hot pot sauce and soup. Noscapine, papaverine, thebaine, and morphine were detected in a positive sample of chicken soup, which was consistent with the result of the HPLC-MS/MS method. This method without sample preparation and chromatographic separation is fast, green, and environmentally benign, thus being suitable for the rapid qualitative analysis of poppy husk in food.

Key words: thermal desorption electrospray ionization (TD-ESI), triple quadruple mass spectrometry (MS/MS), alkaloids, poppy husk, hot pot sauce, soup, rapid detection

ZHANG Hongyan, SHI Xiaofeng, QIU Guoyu, WANG Xiaoqiao, ZHANG Caixia, ZHANG Xiaoping, WU Fuxiang, XU Xiaohui, LI Chenxi, PAN Xiuli. Rapid screening of illegally added poppy husk in hot pot sauce and soup by thermal desorption electrospray ionization-triple quadruple mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(7): 861-867.

Figures/Tables 8

Fig. 1 Principle of thermal desorption (TD)-ESI source

Table 1 CAS Nos., chemical formula, monitoring ions, fragmentor and collision energies (CEs) of five alkaloids

Compound	CAS No.	Chemical formula	Precursor ion (m/z)	Daughter ions (m/z)	Fragmentor/eV	CEs/eV
Noscapine	912-60-7	C₂₂H₂₃NO₇	414.2	220.1, 353.0	120	18, 22
Papaverine	58-74-2	C₂₀H₂₁NO₄	340.2	202.1, 324.1	130	26, 30
Thebaine	115-37-7	C₁₉H₂₁NO₃	312.0	58.2, 251.1	80	10, 26
Codeine	76-57-3	C₁₈H₂₁NO₃	300.2	152.0, 215.1	125	80, 26
Morphine	57-27-2	C₁₇H₁₉NO₃	286.1	128.1, 180.0	130	74, 74

Fig. 2 Effect of different rates of pump on the response intensity Source: TD-ESI, positive; gas temperature: 300 ℃; gas flow: 3 L/min; nebulizer: 34.5 kPa; capillary: 4000 V; temperature of thermal desorption: 260 ℃; solvent of injection: 0.1% formic acid aqueous solution containing 10 mmol/L formic ammonium-acetonitrile (1:1, v/v).

Table 2 LODs for the five alkaloids

Compound	LODs/(μg/kg)
Compound	Hot pot sauce	Soup
Noscapine	2.0	2.0
Papaverine	2.0	2.0
Thebaine	2.0	2.0
Codeine	10.0	5.0
Morphine	10.0	5.0

Fig. 3 MRM spectra of a mixture of the five alkaloid standards in soup by six repetitive test Rate of injection: 200 μL/h; other conditions are the same as those in Fig. 2.

Fig. 4 Results of the five alkaloids in different contents tested by colloidal gold card

Fig. 5 Detection results of the real samples Conditions are the same as those in Fig. 3.

Table 3 Comparison for the five alkaloids tested with different methods

Compound	Results
Compound	TD-ESI-MS/MS	LC-MS/MS/(μg/kg)
Noscapine	positive	56.4
Papaverin	positive	30.1
Thebaine	positive	91.1
Codeine	positive	622
Morphine	negative	not detected

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