Simultaneous Determination of Residues of 23 Plant Growth Regulators in Codonopsis Radix and Angelica Sinensis by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘 要
样品经晾干、粉碎、过筛后,分取3.0 g,加入1.0%(体积分数)冰乙酸溶液5 mL,涡旋,使样品完全浸湿。浸泡30 min后加入乙腈15 mL,剧烈振摇10 min,加入无水硫酸镁(AMS)4.0 g和氯化钠1.0 g,剧烈摇散,防止盐结块,再剧烈振摇10 min,离心10 min。收集全部上清液,于40℃氮吹至近干,残渣用50%(体积分数)乙腈溶液1 mL复溶。所得溶液进入超高效液相色谱-串联质谱仪,其中的目标物在Waters AQUITY UPLC BEH Shield RP18色谱柱上用不同体积比的含5 mmol·L-1甲酸铵的0.05%(体积分数,下同)甲酸溶液以及含5 mmol·L-1甲酸铵和0.05%甲酸的乙腈溶液的混合溶液梯度洗脱分离,采用电喷雾离子源正(ESI+)、负(ESI-)离子模式电离,保留时间依赖多反应监测(sMRM)模式检测,基质匹配法定量。结果显示:23种植物生长调节剂的质量浓度均在一定范围内与对应的峰面积呈线性关系,测定下限(10S/N)为0.2~3.0 μg·kg-1;按照标准加入法进行回收试验,回收率为75.2%~109%,测定值的相对标准偏差(n=5)为1.8%~13%;方法用于46批党参和30批当归样品的分析,其中有10.9%的党参样品和6.7%的当归样品中的4-硝基苯酚钠检出量超过了GB 2763-2021规定的限量(100 μg·kg-1)。
Abstract
After the sample was dried, crushed, and sieved, an aliquot (3.0 g) was taken, and 5 mL of 1.0% (volume fraction) glacial acetic acid solution was added to completely immerse the sample by vortex. After soaking for 30 min, 15 mL of acetonitrile was added, and the mixture was shaken vigorously for 10 min. Then 4.0 g of anhydrous magnesium sulfate (AMS) and 1.0 g of sodium chloride were added, and the mixture was shaken vigorously to prevent salt agglomeration, shaken vigorously for another 10 min, and centrifuged for 10 min. All the supernatant was collected, and blown to near dryness by nitrogen at 40℃, and the residue was dissolved in 1 mL of 50% (volume fraction) acetonitrile solution. The obtained solution was introduced into the ultra-high performance liquid chromatograph-tandem mass spectrometer, and the targets were separated on the Waters AQUITY UPLC BEH Shield RP18 chromatographic column by gradient elution with mixed solutions composed of 0.05% (volume fraction, the same below) formic acid solution containing 5 mmol·L-1 ammonium formate and acetonitrile solution containing 5 mmol·L-1 ammonium formate and 0.05% formic acid at different volume ratios, and ionized by the ESI+ and ESI- modes, detected by the sMRM mode, and quantified by matrix matching method. It was shown that linear relationships between values of the mass concentration and the corresponding peak area of 23 plant growth regulators were kept in definite ranges, with lower limits of determination (10S/N) in the range of 0.2-3.0 μg·kg-1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 75.2%-109%, and RSDs (n=5) of the determined values ranged from 1.8% to 13%. The proposed method was used for the analysis of 46 batches of Codonopsis Radix and 30 batches of Angelica sinensis samples. Among them, detection amounts of sodium 4-nitrophenol in 10.9% of Codonopsis Radix samples and 6.7% of Angelica sinensis samples exceeded the limit (100 μg·kg-1) specified in GB 2763-2021.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202311010
所属栏目 工作简报
基金项目 国家中药及饮片质量控制重点实验室项目(2021GSMPA-KL06)
收稿日期 2022/11/21
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备注刘志荣,工程师,硕士,主要从事药品质量研究
引用该论文: LIU Zhirong,ZHANG Mingtong,MA Xiao,XIE Nan,GUO Zhaohui,DU Haijuan. Simultaneous Determination of Residues of 23 Plant Growth Regulators in Codonopsis Radix and Angelica Sinensis by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(11): 1303~1310
刘志荣,张明童,马潇,谢楠,郭朝晖,杜海娟. 超高效液相色谱-串联质谱法同时测定党参和当归中23种植物生长调节剂的残留量[J]. 理化检验-化学分册, 2023, 59(11): 1303~1310
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【2】ZHOU X, LI R Q, WANG C, et al. Simultaneous quantitation of cytokinin bases and their glycoconjugates with stable isotope labelling ultrahigh performance liquid chromatography mass spectrometry[J]. Journal of Chromatography A, 2021,1636:461782.
【3】PU C H, LIN S K, CHUANG W C, et al. Modified QuEChERS method for 24 plant growth regulators in grapes using LC-MS/MS[J]. Journal of Food and Drug Analysis, 2018,26(2):637-648.
【4】TODESCHINI V, AITLAHMIDI N, MAZZUCCO E, et al. Impact of beneficial microorganisms on strawberry growth, fruit production, nutritional quality, and volatilome[J]. Frontiers in Plant Science, 2018,9:1611.
【5】HAC-WYDRO K, FLASIHSKI M. The studies on the toxicity mechanism of environmentally hazardous natural (IAA) and synthetic (NAA) auxin-The experiments on model Arabidopsis thaliana and rat liver plasma membranes[J]. Colloids and Surfaces B:Biointerfaces, 2015,130:53-60.
【6】WANG L H, WANG M Y, YAN H Y, et al. A new graphene oxide/polypyrrole foam material with pipette-tip solid-phase extraction for determination of three auxins in papaya juice[J]. Journal of Chromatography A, 2014,1368:37-43.
【7】KARADENIZ A, KAYA B, SAVAS B, et al. Effects of two plant growth regulators, indole-3-acetic acid and β-naphthoxyacetic acid, on genotoxicity in drosophila smart assay and on proliferation and viability of HEK293 cells from the perspective of carcinogenesis[J]. Toxicology and Industrial Health, 2011,27(9):840-848.
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【9】魏赫,金红宇,王莹,等.超高效液相色谱-串联质谱法同时测定中药材中23种植物生长调节剂残留量[J].中草药, 2017,48(8):1653-1660.
【10】ZHAO X S, MU Y, YANG M H. A simple multi-residue method for determination of plant growth retardants in Ophiopogon japonicus and soil using ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chemosphere, 2018,207:329-336.
【11】SUTCHARITCHAN C, MIAO S, LI W T, et al. High performance liquid chromatography-tandem mass spectrometry method for residue determination of 39 plant growth regulators in root and rhizome Chinese herbs[J]. Food Chemistry, 2020,322:126766.
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