CN112730690A - 一种有效降低水中硫酸黏菌素残留量的方法 - Google Patents
一种有效降低水中硫酸黏菌素残留量的方法 Download PDFInfo
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Abstract
本发明涉及药物分析领域,具体涉及一种有效降低水中硫酸黏菌素残留量的方法,本发明主要优选了硫酸黏菌素降解的高铁酸钾用量、pH、时间,并对最佳降解条件下废水中腐植酸对降解的影响以及降解产物的抗菌活性、对发光细菌的毒性等进行评价,以有效安全地降解硫酸黏菌素,减少其在环境中的残留,从而减小其诱导或促进环境中质粒介导的耐药基因mcr‑1的产生和传播,从而保障其作为治疗耐药性革兰氏阴性菌感染的最后一道防线的地位。
Description
技术领域
本发明涉及药物分析领域,具体涉及一种有效降低水中硫酸黏菌素残留 量的方法。
背景技术
硫酸黏菌素(Colistin sulfate)是黏菌素的硫酸盐,是唯一允许用于畜禽 生产的多粘菌素药物,为白色或近白色粉末,无臭、味苦,并有引湿性,易 溶于水,微溶于甲醇、乙醇,不溶于丙酮、乙醚等,游离碱微溶于水,在pH3.5~ 7范围内稳定。具有较强的抗革兰氏阴性杆菌作用,尤其对多重耐药革兰氏阴 性致病菌有特效,还具有抗内毒素和促进动物生长的作用,且在动物体内低 残留,因此受到畜牧兽医工作者的青睐,被中国、美国、欧盟、日本等许多 国家批准作为饲料添加剂或兽药。
过去认为,黏菌素的耐药机制仅为染色体突变介导,并不能通过基因的 水平转移引起耐药,因此不易引起耐药基因的广泛快速传播。2015年,研究 者发现了质粒介导的黏菌素耐药基因mcr-1(Mobilecolistin resistance),并证 明了该基因可在不同菌种间传播。由于质粒能够自我复制和在细菌间转移, 引起mcr-1基因的快速传播,这将使多粘菌素类药物耐药性迅速发展,威胁该 类药物作为“最后一道防线”的有效性。
目前,仍有不少国家允许硫酸黏菌素用作饲料添加剂,主要通过口服给 药,其在胃肠道不易吸收,几乎全部以原形随动物粪便排出进入到环境中。 而环境中残留的硫酸黏菌素可能促进mcr-1基因在环境中的产生和传播,给人 类健康带来巨大威胁。但目前关于硫酸黏菌素的降解方法及后续降解产物的 生态毒性评价尚未见报道。因此,寻找一种安全、有效的方法对水中硫酸黏 菌素进行降解对于保障人类安全具有非常重要的意义。高铁酸盐集氧化、絮 凝、消毒于一体,具有强氧化性、反应迅速、无毒副作用等优点,是一种绿色、高效的水处理剂。
发明内容
本发明的目的在于提供一种有效降低水中硫酸黏菌素残留量的方法,所 述方法包括以下步骤:
(1)硫酸黏菌素的降解
精确称量硫酸黏菌素,以纯水为溶剂配置成30μmol/L溶液,按照高铁酸 钾与硫酸黏菌素的摩尔比称取高铁酸钾,用硼砂-磷酸氢二钠缓冲液高铁酸钾 溶液,加入10mL高铁酸钾于离心管中,调节pH,反应一段时间,转速500 rpm,25℃进行降解反应,每组重复3次,反应完后取0.8mL反应液和0.2mL 0.1mol/L硫代硫酸钠置于EP管中,混匀、过柱,待检测;
(2)降解产物的检测
采用Acquity I-Class/Xevo TQS超高效液相色谱串联三重四级杆质谱仪进 行检测:
色谱条件:色谱柱:150mm×2.0mm,3.0μm TSKgel Amide-80;柱温: 40℃;进样量:10μL;流速:0.6mL·min-1;流动相:A 0.1%甲酸水溶液和B 乙腈。梯度洗脱程序:0~0.8min,5%A;0.8~1.5min,5%~80%A;1.5~ 3.0min,80%A;3.0~3.5min,80%~5%A;3.6~5min,5%A;
质谱条件:离子源:电喷雾电离;扫描方式:正离子扫描;离子源温度: 120℃;毛细管电压:3.0kV;脱溶剂气温度:400℃;脱溶剂气流量:950L·h-1; 碰撞气流速:0.15mL·min-1,锥孔反吹气流量:150L·h-1;监测方式:多反应 监测。
优选的,所述步骤(1)中高铁酸钾与硫酸黏菌素摩尔比为30:1。
优选的,所述步骤(1)中反应液pH值为7。
优选的,所述步骤(1)中反应时间为60min。
优选的,所述硫酸黏菌素的降解率为99.9%。
与现有技术相比,本发明的有益效果是:本发明主要优选了硫酸黏菌素 降解的高铁酸钾用量、pH、时间,并对最佳降解条件下废水中腐植酸对降解 的影响以及降解产物的抗菌活性、对发光细菌的毒性等进行评价,以有效安 全地降解硫酸黏菌素,减少其在环境中的残留,从而减小其诱导或促进环境 中质粒介导的耐药基因mcr-1的产生和传播,保障其作为治疗耐药性革兰氏阴 性菌感染的最后一道防线的地位。
附图说明
图1为黏菌素定量离子对MRM质量色谱图,CSA和CSB分别为黏菌素 A和黏菌素B;
图2为最佳条件下采用高铁酸钾降解硫酸黏菌素对大肠杆菌ATCC 25922、大肠杆菌k88,金黄色葡萄球菌及枯草芽孢杆菌的抗菌等效值;
图3为硫酸黏菌素及其在最佳条件下高铁酸钾降解的产物对费氏弧菌的 发光毒性。
具体实施方式
下面结合实例对本发明进行进一步的说明。
实施例1
硫酸黏菌素的降解
(1)高铁酸钾用量对硫酸黏菌素降解的影响
精确称量硫酸黏菌素,以纯水为溶剂配置成30μmol/L溶液。依据高铁酸 钾与硫酸黏菌素摩尔比:5倍(150μmol/L),10倍(300μmol/L),20倍(600 μmol/L),30倍(900μmol/L),40倍(1200μmol/L)称取高铁酸钾,用硼 砂-磷酸氢二钠缓冲液分别配置相应浓度高铁酸钾溶液。取硫酸黏菌素10mL+ 高铁酸钾10mL于离心管中,以条件:pH=9,反应时间60min,转速500rpm, 25℃进行降解反应(每个摩尔比倍数重复3次)。反应完后取0.8mL反应液+0.2 mL0.1mol/L硫代硫酸钠置于EP管中,混匀、过柱,待检测。
(2)pH对硫酸黏菌素降解的影响
称量相应的硫酸黏菌素用纯水配置成30μmol/L溶液。优选出来的高铁酸 钾与硫酸黏菌素摩尔比倍数配置高铁酸钾溶液。取硫酸黏菌素10mL+高铁酸 钾10mL以反应时间60min,转速500rpm,25℃,不同pH值:5,6,7,8,9, 10为反应条件进行降解反应(每个pH值3次重复)。反应完后取0.8mL反应液 +0.2mL 0.1mol/L硫代硫酸钠置于EP管中,混匀、过柱,待检测。
(3)反应时间对降解效果的影响
称量相应的硫酸黏菌素用纯水配置成30μmol/L溶液。优选出来的高铁酸 钾浓度(高铁酸钾与硫酸黏菌素摩尔比倍数)。取硫酸黏菌素10mL+高铁酸 钾10mL,以条件:转速500rpm,25℃,优选出来的pH值,不同反应时间: 30s,1,2,5,10,15,30,45,60min进行降解反应(每个时间段3次重复)。 反应完后取0.8mL反应液+0.2mL 0.1mol/L硫代硫酸钠置于EP管中,混匀、 过柱,待检测。
(4)腐植酸对硫酸黏菌素降解的影响
称适量硫酸黏菌素,用纯水配制成30μmol/L溶液。优选出来的高铁酸钾 浓度(高铁酸钾与硫酸黏菌素摩尔比倍数)。称取相应质量的腐植酸加入10mL 硫酸黏菌素溶液中形成腐植酸浓度分别为0,1,5,15,30,60mg/L的溶液; 在其中加入高铁酸钾10mL,以转速500rpm,25℃,优选出来的时间,优选 出来的pH为条件进行降解反应(每个腐植酸浓度3次重复)。反应完后取0.8 mL反应液+0.2mL 0.1mol/L硫代硫酸钠置于EP管中,混匀、过柱,待检测。
仪器:Acquity I-Class/Xevo TQS超高效液相色谱串联三重四级杆质谱仪 (美国Waters公司);色谱条件:色谱柱:TSKgel Amide-80(150mm×2.0mm, 3.0μm);柱温:40℃;进样量:10μL;流速:0.6mL·min-1;流动相:0.1% 甲酸水溶液(A)和乙腈(B)。梯度洗脱程序:0~0.8min,5%A;0.8~1.5 min,5%~80%A;1.5~3.0min,80%A;3.0~3.5min,80%~5%A;3.6~5 min,5%A。
质谱条件:离子源:电喷雾电离(ESI);扫描方式:正离子扫描;离子源温 度:120℃;毛细管电压:3.0kV;脱溶剂气温度:400℃;脱溶剂气流量: 950L·h-1;碰撞气流速:0.15mL·min-1,锥孔反吹气流量:150L·h-1;监测 方式:多反应监测(multiple-periodMRM),结果如表1所示。
表1目标分析物MRM质谱采集参数1)
注:1)*表示定量离子;CSA和CSB分别为黏菌素A和黏菌素B。
从表2中数据得出腐植酸的存在对最佳条件下高铁酸钾降解硫酸黏菌素 无明显影响,差异不显著(p>0.05)。
表2腐植酸的存在对高铁酸钾降解硫酸黏菌素的影响
a.将使用调和均值样本大小=3.000。
实施例2
抗菌活性及降解产物的发光细菌毒性
采用微量倍比稀释法进行抗菌活性测定;按ISO-11348-3标准中所述方法, 采用费氏弧菌进行发光毒性测试。
采用等效值(potency equivalent quotient,PEQ)评价降解产物抗菌活性 的变化,其公式为:PEQ=EC50(CS0)/EC50(CSt),其中,EC50(CS0)和EC50(CSt) 分别为硫酸黏菌素降解前和降解后的半数抑菌浓度。PEQ<1,说明降解产物 抗菌活性低于母药。结果如图3所示,所有受试菌的PEQ均小于1,说明硫酸 黏菌素在最佳条件下用高铁酸钾进行降解可有效降低其对环境微生物的影 响。
硫酸黏菌素及其降解产物对费氏弧菌发光的抑制率IR%分别为7.38%和2.99%,均远低于30%,说明二者对费氏弧菌均无明显毒性,且经过高铁酸钾降 解后,其毒性进一步降低。证明采用该法对水质具有较好的安全性,结果如 图3。
硫酸黏菌素初始浓度为30μmol/L时,高铁酸钾与硫酸黏菌素投加摩尔比 为30,反应液pH值为7,反应60min,降解率已达99.9%;腐植酸对高铁酸钾降 解硫酸黏菌素无显著影响;硫酸黏菌素在最佳条件下用高铁酸钾进行降解可 有效降低其对环境微生物的影响;且原药及产物对水质均无显明毒性。
Claims (5)
1.一种有效降低水中硫酸黏菌素残留量的方法,其特征在于:所述方法包括以下步骤:
(1)硫酸黏菌素的降解
精确称量硫酸黏菌素,以纯水为溶剂配置成30μmol/L溶液,按照高铁酸钾与硫酸黏菌素的摩尔比称取高铁酸钾,用硼砂-磷酸氢二钠缓冲液高铁酸钾溶液,加入10mL高铁酸钾于离心管中,调节pH,反应一段时间,转速500rpm,25℃进行降解反应,每组重复3次,反应完后取0.8mL反应液和0.2mL 0.1mol/L硫代硫酸钠置于EP管中,混匀、过柱,待检测;
(2)降解产物的检测
采用AcquityI-Class/Xevo TQS超高效液相色谱串联三重四级杆质谱仪进行检测:
色谱条件:色谱柱:150mm×2.0mm,3.0μm TSKgel Amide-80;柱温:40℃;进样量:10μL;流速:0.6mL·min-1;流动相:A 0.1%甲酸水溶液和B乙腈。梯度洗脱程序:0~0.8min,5%A;0.8~1.5min,5%~80%A;1.5~3.0min,80%A;3.0~3.5min,80%~5%A;3.6~5min,5%A;
质谱条件:离子源:电喷雾电离;扫描方式:正离子扫描;离子源温度:120℃;毛细管电压:3.0kV;脱溶剂气温度:400℃;脱溶剂气流量:950L·h-1;碰撞气流速:0.15mL·min-1,锥孔反吹气流量:150L·h-1;监测方式:多反应监测。
2.根据权利要求1所述方法,其特征在于:所述步骤(1)中高铁酸钾与硫酸黏菌素摩尔比为30:1。
3.根据权利要求1所述方法,其特征在于:所述步骤(1)中反应液pH值为7。
4.根据权利要求1所述方法,其特征在于:所述步骤(1)中反应时间为60min。
5.根据权利要求1-4任一所述方法,其特征在于:所述硫酸黏菌素的降解率为99.9%。
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