超高效液相色谱-串联质谱法测定蛇毒及蛇毒血凝酶制剂中38种药物残留  

Determination of 38 Kinds of Drug Residues in Venin and Hemocoagulase Preparations by UPLC-MS/MS

作　　者：唐娜 王建山 宋莉 田美虹 王嫦鹤 TANG Na;WANG Jianshan;SONG Li;TIAN Meihong;WANG Changhe(Shaanxi Institute for Food and Drug Control,Xi'an,Shaanxi,China 710065)

机构地区：[1]陕西省食品药品检验研究院,陕西西安710065

出　　处：《中国药业》2025年第3期71-75,共5页China Pharmaceuticals

摘　　要：目的建立测定蛇毒及蛇毒血凝酶制剂中38种药物残留量的超高效液相色谱-串联质谱法。方法采用电喷雾正/负离子和多反应监测模式扫描,以0.1%甲酸-0.5 mmol/L乙酸铵水溶液-乙腈为流动相(梯度洗脱),采用Waters Cortecs T3色谱柱(100 mm×2.1 mm,2.7μm)进行分离。结果38种药物在各自质量浓度范围内与峰面积线性关系良好(r>0.994,n=6);精密度、稳定性试验结果的RSD均小于4.00%(n=6);低、中、高质量浓度的加样回收率分别为78.34%~90.52%、83.61%~105.33%、88.21%~108.50%,RSD分别为2.51%~7.33%、0.84%~5.73%、1.21%~4.94%(n=3)。采用该方法检测了4批蛇毒血凝酶制剂和3种蛇毒中38种药物的残留情况,结果均未检出大环内酯类、磺胺类、喹诺酮类抗菌药物,符合相关要求,但在1批蛇毒中检出了17.2 ng/g氯霉素类抗菌药物氟甲砜霉素残留。结论该方法操作简便、重复性好、结果准确,适用于蛇毒及蛇毒血凝酶制剂中38种药物残留量的检测,可为蛇毒血凝酶类产品的质量控制提供参考。Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of drug residues in venin and hemocoagulase preparations.Methods The electrospray positive/negative ion and multi reaction monitoring mode were adopted for scanning.0.1%formic acid-0.5 mmol/L ammonium acetate aqueous solution-acetonitrile was used as mobile phase(gradient elution),and Waters Cortecs T3 chromatographic column(100 mm×2.1 mm,2.7μm)was used for separation.Results A total of 38 drugs showed good linear relationship with peak area within their respective mass concentration ranges(r>0.994,n=6).The recovery rates of low-,medium-,and high-quality concentrations were in the ranges of 78.34%-90.52%,83.61%-105.33%,and 88.21%-108.50%,with RSDs of 2.51%-7.33%,0.84%-5.73%,and 1.21%-4.94%(n=3),respectively.This method was used to detect the residues of 38 drugs in four batches of hemocoagulase preparations and three types of venin.The results showed that no macrolides,sulfonamides,or quinolone antibiotics were detected,which could meet the relevant requirements.However,17.2 ng/g of chloramphenicol antibiotics(florfenicol)residue was detected in one batch of venin.Conclusion This method is simple,sensitive,reproducible,and accurate,which is suitable for the determination of 38 kinds of drug residues in venin and hemocoagulase preparations,and can provide a reference for the quality control of hemocoagulase preparations.

关 键 词：超高效液相色谱-串联质谱法 蛇毒 蛇毒血凝酶制剂 药物残留 

分 类 号：R917[医药卫生—药物分析学]