首页|期刊导航|中国兽医杂志|牛血浆中莫昔克丁和三氯苯达唑LC-MS/MS检测方法的建立与验证

牛血浆中莫昔克丁和三氯苯达唑LC-MS/MS检测方法的建立与验证OA

Establishment and Validation of LC-MS/MS Detection Method for Moxidectin and Triclabendazole in Bovine Plasma

中文摘要英文摘要

为同步测定牛血浆中的莫昔克丁(MOX)、三氯苯达唑(TCB)及其代谢物三氯苯达唑亚砜(TCB-SO)和三氯苯达唑砜(TCB-SO2),本试验建立了一种液相色谱-串联质谱(LC-MS/MS)方法,并对该方法的特异性、线性范围、检测限(LOD)、定量限(LOQ)、基质效应、回收率、精密度、稀释效应和稳定性进行验证.结果显示,本试验建立的用于同步测定牛血浆中MOX、TCB及其代谢物的方法具有良好的特异性.MOX(0.25~20.00 ng/mL)、TCB(5~500 ng/mL)、TCB-SO(50~5 000 ng/mL)和TCB-SO₂(50~5 000 ng/mL)在各自的线性范围内均呈现良好线性,决定系数(R2)均超过0.990 000.MOX、TCB、TCB-SO和TCB-SO₂的LOD分别为0.125、2.5、25和25 ng/mL,LOQ分别为0.250、5.0、50和50 ng/mL.低、高浓度样品内标归一化基质因子的变异系数(CV)分别为0.85%~13.65%和2.09%~6.26%,均小于15%.牛血浆中4种目标化合物的批内回收率均大于92%,批间回收率均大于97%,批内精密度均小于8%,批间精密度均小于7%.稀释后的血浆基质标准品中,4种目标化合物的批间CV均小于8.00%.此外,该方法稳定性良好,血浆基质样品在长期冻存、反复冻融、室温放置、进样盘放置等条件下浓度偏差均小于15.00%.结果表明,本试验建立的LC-MS/MS方法稳定、可靠,可用于牛血浆中MOX、TCB及其代谢物的同步测定.

To simultaneously determine moxidectin(MOX),triclabendazole(TCB),and its metabolites triclabendazole sulphoxide(TCB-SO)and triclabendazole sulphone(TCB-SO₂)in bovine plasma,an ultra-performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was developed and validated for specificity,linearity,limit of detection(LOD),limit of quantification(LOQ),matrix effect,recovery,precision,dilution effect,and stability.The results showed that the developed method exhibited good specificity for the simultaneous determination of MOX,TCB,and their metabolites in bovine plasma.MOX(0.25-20.00 ng/mL),TCB(5-500 ng/mL),TCB-SO(50-5 000 ng/mL),and TCB-SO₂(50-5 000 ng/mL)showed good linearity within their respective ranges,with correlation coefficients(R²)all exceeding 0.990 000.The LODs of MOX,TCB,TCB-SO,and TCB-SO₂ were 0.125,2.5,25,and 25 ng/mL,respectively,and the LOQs were 0.250,5.0,50,and 50 ng/mL,respectively.The coefficient of variation(CV)of the internal standard-normalized matrix factors for low-and high-concentration samples were 0.85%-13.65%and 2.09%-6.26%,respectively,all below 15%.The intra-batch recoveries of the four target compounds in bovine plasma were all above 92%,and the inter-batch recoveries were all above 97%.The intra-batch precision was less than 8%,and the inter-batch precision was less than 7%.For diluted plasma matrix standards,the inter-batch CVs of all four target compounds were below 8.00%.In addition,the method showed good stability,with concentration deviations of less than 15.00%under conditions of long-term freezing,repeated freeze-thaw cycles,room temperature storage,and autosampler storage.These results indicate that the established LC-MS/MS method is stable and reliable and can be used for the simultaneous determination of MOX,TCB,and their metabolites in bovine plasma.

吴煜锋;张梦迪;陈婷婷;郎丰亭;金科旭;李凯歌;郝智慧

新疆农业大学动物医学学院,新疆 乌鲁木齐 830052中国农业大学动物医学院,北京 海淀 100193中国农业大学动物医学院,北京 海淀 100193新疆农业大学动物医学学院,新疆 乌鲁木齐 830052新疆农业大学动物医学学院,新疆 乌鲁木齐 830052新疆农业大学动物医学学院,新疆 乌鲁木齐 830052中国农业大学动物医学院,北京 海淀 100193

农业科技

莫昔克丁(MOX)三氯苯达唑(TCB)液相色谱-串联质谱(LC-MS/MS)牛血浆

moxidectin(MOX)triclabendazole(TCB)liquid chromatography-tandem mass spectrometry(LC-MS/MS)bovine plasma

《中国兽医杂志》 2026 (6)

61-69,9

国家重点研发计划(2022YFD1801105)

10.20157/j.cnki.zgsyzz.2026.06.008

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