Boison Joe O, Lee Stephen, Matus Johanna
Centre for Veterinary Drug Residues, Canadian Food Inspection Agency (CVDR), Saskatoon Laboratory, 116 Veterinary Road, Saskatoon, Saskatchewan, S7N 2R3, Canada,
Anal Bioanal Chem. 2015 May;407(14):4065-78. doi: 10.1007/s00216-015-8644-z. Epub 2015 Apr 2.
A new multi-residue method for the determination of seven polypeptides, namely, polymixin B1, polymixin B2, polymixin E1 (colistin A), polymixin E2 (colistin B), enduracidin A (enramycin A), enduracidin B (enramycin B), and bacitracin A, in food of animal origin was developed and validated for chicken muscle tissue. Chicken muscle tissue was extracted with acidified methanol (1 % TFA). After homogenization, shaking, and centrifugation, the acidified methanol extract was decanted. A second extraction was performed with methanol (1 % TFA) and formic acid (1 %) 25:75, v/v. The pooled extract was cleaned up and concentrated on a solid-phase extraction cartridge. The retained analytes were eluted with methanol/acetonitrile. The extract was evaporated to dryness, reconstituted in mobile phase, filtered, and quantified by LC-MS/MS under ESI conditions. The method has a LOQ of 50.0 μg/kg for polymixin E2 (colistin B), 39.0 μg/kg for polymixin E1 (colistin A), 74.0 μg/kg for polymixin B1, 71.0 μg/kg for polymixin B2, 66.0 μg/kg for enduracidin A, 50.0 μg/kg for enduracidin B, and 30.0 μg/kg for bacitracin A in chicken muscle tissues. This is the first sensitive, suitable, multi-residue method reported for the seven polypeptide drug residues in chicken muscle tissue.
建立了一种用于测定动物源性食品中7种多肽（即多粘菌素B1、多粘菌素B2、多粘菌素E1（黏菌素A）、多粘菌素E2（黏菌素B）、持久霉素A（恩拉霉素A）、持久霉素B（恩拉霉素B）和杆菌肽A）的新型多残留方法，并在鸡肉组织中进行了验证。鸡肉组织用酸化甲醇（1%三氟乙酸）提取。匀浆、振荡和离心后，倾析出酸化甲醇提取物。用甲醇（1%三氟乙酸）和甲酸（1%）按体积比25:75进行第二次提取。合并提取物在固相萃取柱上进行净化和浓缩。保留的分析物用甲醇/乙腈洗脱。提取物蒸发至干，用流动相复溶，过滤，并在电喷雾电离（ESI）条件下通过液相色谱-串联质谱（LC-MS/MS）进行定量。该方法在鸡肉组织中对多粘菌素E2（黏菌素B）的定量限为50.0μg/kg，对多粘菌素E1（黏菌素A）为39.0μg/kg，对多粘菌素B1为74.0μg/kg，对多粘菌素B2为71.0μg/kg，对持久霉素A为66.0μg/kg，对持久霉素B为50.0μg/kg，对杆菌肽A为30.0μg/kg。这是首次报道的用于鸡肉组织中7种多肽药物残留的灵敏、适用的多残留方法。
