|
|
|
| Determination of three tropane alkaloids in infant foods by liquid chromatography-tandem mass spectrometry |
| WU Hao1, XU Meijia2, XU Jiaojiao2, AN Yuxin2, HAN Jianlong2, XU Xiaomin2,3,4
|
1. School of Public Health, Hangzhou Medical College, Hangzhou, Zhejiang 311399, China;
2. NHC Specialty Laboratory of Food Safety Risk Assessment and Standard Development, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, Zhejiang 310051, China;
3. Zhejiang Key Laboratory of Public Health Detection and Pathogenesis Research, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, Zhejiang 310051, China;
4. Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, Zhejiang 310051, China |
|
|
|
|
Abstract Objective To establish a method for the determination of anisodamine, atropine, and scopolamine in infant complementary foods and formula milk powder by solid-phase extraction combined with liquid chromatography-tandem mass spectrometry. Methods Commercially available infant complementary foods (biscuits, noodles, and rice flour) and formula milk powder were collected. The samples were homogenized, extracted ultrasonically with 0.5% formic acid-80% aqueous methanol solution, and purified using polymer-based mixed-mode cation-exchange solid-phase extraction cartridges. Gradient elution was performed with 0.02% formic acid-1 mmol/L ammonium formate aqueous solution and methanol as mobile phases. The target compounds were separated using an XBridgeTM BEH C18 column (150 mm×3 mm, 2.5 μm), detected by positive electrospray ionization multiple reaction monitoring mode, and quantified using the isotope internal standard method. Results When 0.5% formic acid-80% aqueous methanol solution was used for extraction and the loading volume was 5 mL, the peak areas and average spiked recovery rates of the target compounds were relatively high. The matrix effects of infant food were evaluated using the optimized method. Noodles showed a matrix suppression effect, whereas biscuits, rice flour, and formula milk powder exhibited matrix effects close to 100%, which were corrected by isotope internal standard quantification. The three tropane alkaloids had good linear relationships in the range of 0.1-50 ng/mL, with all correlation coefficients greater than 0.999. The limits of detection and limit of quantification were 0.1 and 0.3 μg/kg, respectively. At spiked concentrations of 0.3, 8.0, and 40.0 μg/kg, the average spiked recovery rates of anisodamine, atropine, and scopolamine were 95.7%-102.6%, 93.2%-104.7%, and 95.5%-104.1%, respectively, with relative standard deviations of 1.4%-8.5%, 1.5%-8.4%, and 3.1%-8.5%, respectively. None of the three tropane alkaloids were detected in 100 infant complementary food samples. Among 60 infant formula milk powder samples, atropine and scopolamine were detected in one sample, while anisodamine was not detected. Conclusions The method is simple, accurate, and sensitive, and can effectively eliminate the interference of complex matrix effects. It can be applied to the quantitative determination of tropane alkaloids in infant foods.
|
|
Received: 27 April 2026
Revised: 29 July 2026
Published: 21 August 2026
|
|
|
|
|
|
[1] Sharma M,Dhaliwal I,Rana K,et al.Phytochemistry,pharmacology,and toxicology of Datura species-a review[J/OL].Antioxidants (Basel),2021,10(8)[2026-07-29].https://doi.org/10.3390/antiox10081291.
[2] Kohnen-Johannsen K L,Kayser O.Tropane alkaloids:chemistry,pharmacology,biosynthesis and production[J/OL].Molecules,2019,24(4)[2026-07-29].https://doi.org/10.3390/molecules24040796.
[3] 邓淑铃,朱峰,张昊,等.液相色谱-串联质谱法检测芝麻糊样品中东莨菪碱、消旋山莨菪碱和阿托品[J].化学分析计量,2025(2):18-24.
[4] 李晓华,潘奕夫,韩世明.朔州市一起曼陀罗引起食物中毒事件的调查[J].中国食品卫生杂志,2023,35(3):443-446.
[5] GB2715—2016 食品安全国家标准粮食[S].
[6] European Union.Commission Regulation(EU)2021/1408 of 27 August2021 amending regulation(EC)No 1881/2006 as regards maximum levels of tropane alkaloids in certain foodstuffs(text with EEA relevance)[EB/OL].[2026-07-29].https://eur-lex.europa.eu/eli/reg/2021/1408/oj/eng.
[7] El Bazaoui A,Bellimam M A,Soulaymani A.Nine new tropane alkaloids from Datura stramonium L. identified by GC/MS[J].Fitoterapia,2011,82(2):193-197.
[8] Klein L M,Gabler A M,Rychlik M,et al.A sensitive LC-MS/MS method for isomer separation and quantitative determination of 51 pyrrolizidine alkaloids and two tropane alkaloids in cow's milk[J].Anal Bioanal Chem,2022,414(28):8107-8124.
[9] 邹晓春,陈映新,刘红河.超高效液相色谱-四极杆串联线性离子阱质谱法测定中毒样品中三种曼陀罗生物碱[J].现代预防医学,2025,52(18):3403-3409.
[10] 周荣贵,寇金蟾,张永泓,等.超高效液相色谱-四级杆-飞行时间质谱法快速检测曼陀罗中毒事件中有毒物质[J].中国食品卫生杂志,2025,37(4):327-332.
[11] 邓淑铃,朱峰,张昊,等.液相色谱-串联质谱法测定曼陀罗中东莨菪碱、消旋山莨菪碱和阿托品含量[J].食品安全质量检测学报,2025,16(11):131-139.
[12] 刘峰,张银豪,马明阳,等.液相色谱-串联质谱法检测一起误食曼陀罗引起的食物中毒物质[J].中国食品卫生杂志,2022,34(2):377-381.
[13] 胡侠,付丽莎.液相色谱-串联质谱法同时快速测定婴幼儿谷物食品中3种莨菪烷生物碱[J].大连民族大学学报,2021,23(3):206-210. |
|
|
|
