高效液相色谱-串联质谱法测定河蟹肝胰腺组织中林可酰胺类抗生素残留

邱稀木; 朱晓华; 边文冀; 王淑芳; 孟勇

doi:10.19303/j.issn.1008-0384.2021.10.016

高效液相色谱-串联质谱法测定河蟹肝胰腺组织中林可酰胺类抗生素残留

Determination of Lincosamide Antibiotics Residues in Crab Tissues

摘要

摘要:
目的基于固相萃取技术（SPE），建立一种可靠的高效液相色谱-串联质谱法测定河蟹样品中林可酰胺类抗生素药物的检测方法。
方法以固相萃取柱为样品净化材料，考察其对河蟹肝胰腺样品的净化效果，优化色谱条件和质谱参数，并对方法进行评价。
结果在河蟹肝胰腺基质中，OASIS^® HLB SPE柱对3种药物的回收率最高。以InfinityLab poroshell 120 SB-C₁₈（100 mm×2.7 mm，2.7 μm）柱为固定相，0.1%甲酸水（A相）和甲醇（B相）为流动相，采用多反应监测（MRM）模式对3种林可酰胺类药物进行检测和定量。3种目标药物为50 μg·L⁻¹，方法线性良好，3种药物检出限为0.22～0.35 μg·kg⁻¹，定量限为0.72～1.16 μg·kg⁻¹，相关系数（R²）大于0.99。在添加量为5、10和50 μg·kg⁻¹质量浓度的空白样品加标回收率试验中，3种林可酰胺类药物的绝对回收率为80.5%～99%，相对标准偏差为2.5%～5.2%。
结论本LC-MS/MS方法提供了一种简便快捷的解决方案，以固相萃取技术为切入点，测定河蟹样品中3种林可酰胺类抗生素的残留，具有稳定可靠，重现性好的特点。

Abstract:
Objective An HPLC-MS/MS method following an optimized solid phase extraction (SPE) procedure was established for the determination of lincosamide antibiotics in crab tissues.
Method SPE column was used to separate and purify the substances from crab roe samples. Lincomycin, clindamycin, and pyrimycin were the target antibiotics to be detected by the methodology.
Result Among the tested materials for the chemical separation, OASIS^® HLB SPE column exhibited the highest recovery rate on the antibiotics. For the HPLC-MS/MS determination on the antibiotics, the gradient elution on an Infinity Lab poroshell 120 SB-C₁₈ column (100 mm×2.7 mm, 2.7 μm) using 0.1% formic acid for the mobile phase A and methanol for the mobile phase B under the multi-reaction monitoring mode was applied. A measurement linearity within 50 μg·L⁻¹ with a R²＞0.99 was achieved. The assay performed with a recovery rate ranging 80.5%–99%, the relative standard deviation 2.5%–5.2%, the detection limit 0.22–0.35 μg·kg⁻¹, and the quantitative limit 0.72–1.16 μg·kg⁻¹.
Conclusion The newly established methodology was stable and reliable in detecting the antibiotics in crab at a reduced cost.

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