| 林澍,耿岳,杨昊,王璐,彭祎,邓凯,张景然,刘潇威.超高效液相色谱串联质谱测定果蔬、糖料作物及谷物中春雷霉素的残留[J].农业环境科学学报,2024,43(12):3034-3040. |
| 超高效液相色谱串联质谱测定果蔬、糖料作物及谷物中春雷霉素的残留 |
| Determination of kasugamycin residues in fruits,vegetables,sugar crop,and cereal by ultra-performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2024-01-29 |
| DOI：10.11654/jaes.2024-0112 |
| 中文关键词: 春雷霉素 水果 蔬菜 糖料作物 谷物 超高效液相色谱串联质谱 残留检测 |
| 英文关键词: kasugamycin fruit vegetable sugar crop cereal UPLC-MS/MS residue determination |
| 基金项目:国家农产品质量安全风险评估项目（GJFP2019034）；中国农业科学院科技创新工程项目 |
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| 中文摘要: |
| 建立了测定水果（苹果、葡萄、柑橘）、蔬菜（茄子、普通白菜、黄瓜）、糖料作物（甘蔗）以及谷物（糙米）中春雷霉素残留量的离子色谱柱-超高效液相色谱串联质谱法。试样采用水和0.1 mmol·L-1乙酸水溶液提取，HLB固相萃取柱净化后，经Metrohm Metrosep A Supp 5（4.0 mm×150 mm，5 μm）色谱柱分离，以水和200 mmol·L-1碳酸氢铵+0.05%氨水溶液为流动相进行梯度洗脱，采用正离子电喷雾离子源（ESI+），以多反应监测模式进行串联质谱分析，外标法测定。结果表明，春雷霉素在该试验条件下有较好的保留，且在较宽的质量浓度范围内（0.001/0.002~0.5 mg·L-1）呈现良好的线性关系（R2≥0.991），定量限为0.005~0.010 mg·kg-1。在0.01（苹果为0.005）、0.05、0.1 mg·kg-1和1 mg·kg-1的添加水平下，春雷霉素在各基质中的日间平均回收率（n=15）为81.9%~125.2%，相对标准偏差为7.4%~20.5%。该方法易于操作，灵敏度高，具有良好的回收率与重现性，适用于水果、蔬菜、糖料、谷物等各类农产品中春雷霉素的残留检测。 |
| 英文摘要: |
| A ultra-performance liquid chromatography-tandem mass spectrometry（UPLC-MS / MS）coupled with ion chromatography column method was developed for the determination of kasugamycin residues in fruits（apples, grapes, citrus fruits）, vegetables（aubergines, pak choi, cucumber）, sugar crop（sugar cane）and cereal（brown rice）. The samples were extracted with water and aqueous acetic acid solution, purified on a HLB solid phase extraction column and separated on a Metrohm Metrosep A Supp 5 column（4.0 mm×150 mm, 5 μm）with a gradient elution using water and 200 mmol·L-1 ammonium bicarbonate +0.05% aqueous ammonia solution as mobile phases, and then analysed by a positive electrospray ionisation（ESI+）source in a multiple reaction monitoring mode for tandem mass spectrometry analysis and an external standard method for quantification. The results showed that kasugamycin was well retained under the test conditions and exhibited good linearity（R2≥0.991）over a wide concentration range（0.001/0.002-0.5 mg·L-1）, with limits of quantification （LOQs）of 0.005-0.010 mg·kg-1. The mean inter-day recoveries（n=15）of kasugamycin in each matrix at spiked levels of 0.01（0.005 for apple）, 0.05, 0.1 and 1 mg · kg-1 ranged from 81.9% to 125.2% with relative standard deviations（RSDs）of 7.4% - 20.5%. The present method is simple to use, sensitive and suitable for the determination of kasugamycin residues in various agricultural products such as fruits, vegetables, sugar crop and cereal. |
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