建立了蔬菜中4种喹诺酮类抗生素的超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)分析方法。每克蔬菜样品(干重)以15 mL乙腈-HCl(125∶8,V/V)进行振荡-超声提取3次,用HLB固相萃取柱进行净化富集,以6 mL 1%酸化乙腈进行洗脱,用N2进行吹...建立了蔬菜中4种喹诺酮类抗生素的超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)分析方法。每克蔬菜样品(干重)以15 mL乙腈-HCl(125∶8,V/V)进行振荡-超声提取3次,用HLB固相萃取柱进行净化富集,以6 mL 1%酸化乙腈进行洗脱,用N2进行吹脱,最后用初始流动相进行定容。以0.1%甲酸-乙腈溶液和0.1%甲酸溶液作为流动相,采用梯度洗脱方式进行UPLC-ESI-MS/MS检测。蔬菜中4种喹诺酮类化合物不同浓度加标回收率为61%～90%;相对标准偏差(RSD)小于5%(个别除外);检出限为0.021～0.092μg/kg;定量限为0.065～0.312μg/kg。本方法能够满足实际蔬菜样品的分析要求。展开更多
Development of new self-calibrating fluorescent sensing methods has been a popular research field with the aim of protecting the human health and environment sustainability. In this work, a novel Eu-based metal organi...Development of new self-calibrating fluorescent sensing methods has been a popular research field with the aim of protecting the human health and environment sustainability. In this work, a novel Eu-based metal organic framework(MOF) Eu(2,6-NDC)(COO)(BUC-88) was developed by employing 2,6-NDC(2,6-naphthalenedicarboxylic acid) as bridging ligands. BUC-88 performed different sensing process toward quinolone antibiotics and tetracyclines antibiotics in terms of fluorescence intensity and color. BUC-88exhibited excellent selectivity and sensitivity detection property toward enrofloxacin(ENR), norfloxacin(NOR) and ciprofloxacin(CIP) over other Pharmaceutical and Personal Care Products(PPCPs), accomplishing the detection limit of 0.12 μmol/L, 0.52 μmol/L, 0.75 μmol/L, respectively. Notably, BUC-88 acted as an excellent fluorescence sensor for tetracyclines antibiotics with fast response time(less than 1 s), high selectivity and sensitivity(LODs = 0.08 μmol/L). The fluorescent detection method was successfully used for visual and ultrasensitive detection of ENR, NOR, CIP and tetracycline hydrochloride(TC) in lake water with satisfied recovery from 99.75% to 102.30%. Finally, the photoinduced electron transfer and the competitive absorption of ultraviolet light are the main mechanisms for sensitive detection toward quinolone antibiotics and tetracyclines antibiotics.展开更多
文摘目的:系统评价前列舒通胶囊联合喹诺酮类抗菌药物治疗慢性前列腺炎的疗效与安全性,以为临床提供循证参考。方法:计算机检索Pub Med、EMBase、Cochrane图书馆、中国生物医学文摘数据库、中国期刊全文数据库、中文科技期刊数据库和万方数据库,收集前列舒通胶囊联合喹诺酮类抗菌药物(试验组)对比单用喹诺酮类抗菌药物(对照组)治疗慢性前列腺炎的随机对照试验(RCT),对符合纳入标准的临床研究进行资料提取,并采用改良后的Jadad量表进行质量评价,采用Rev Man 5.3统计软件进行Meta分析。结果:共纳入16项RCT,合计2 368例患者。Meta分析结果显示,试验组患者的总有效率[RR=1.56,95%CI(1.29,1.88),P<0.001]、美国国立卫生研究院慢性前列腺炎症状指数评分[MD=-6.97,95%CI(-8.67,-5.26),P<0.001]、疼痛症状评分[MD=-3.18,95%CI(-3.92,-2.44),P<0.001]、排尿障碍评分[MD=-1.62,95%CI(-1.85,-1.38),P<0.001]、生活质量评分[MD=-2.16,95%CI(-2.89,-1.43),P<0.001]、前列腺液白细胞计数[MD=-8.90,95%CI(-11.79,-6.02),P<0.001]和复发率[RR=0.22,95%CI(0.12,0.42),P<0.001]均显著优于对照组,差异均有统计学意义;两组患者不良反应发生率比较,差异无统计学意义[RR=0.49,95%CI(0.11,2.13),P=0.34]。结论:前列舒通胶囊联合喹诺酮类抗菌药物治疗慢性前列腺炎的疗效优于单用喹诺酮类抗菌药物,安全性相当。
文摘建立了蔬菜中4种喹诺酮类抗生素的超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)分析方法。每克蔬菜样品(干重)以15 mL乙腈-HCl(125∶8,V/V)进行振荡-超声提取3次,用HLB固相萃取柱进行净化富集,以6 mL 1%酸化乙腈进行洗脱,用N2进行吹脱,最后用初始流动相进行定容。以0.1%甲酸-乙腈溶液和0.1%甲酸溶液作为流动相,采用梯度洗脱方式进行UPLC-ESI-MS/MS检测。蔬菜中4种喹诺酮类化合物不同浓度加标回收率为61%～90%;相对标准偏差(RSD)小于5%(个别除外);检出限为0.021～0.092μg/kg;定量限为0.065～0.312μg/kg。本方法能够满足实际蔬菜样品的分析要求。
基金supported by National Natural Science Foundation of China (Nos. 51878023 and 21806008)Beijing Talent Project (No. 2020A27)The Fundamental Research Funds for Beijing University of Civil Engineering and Architecture (No.X20147/X20141/X20135/X20146)。
文摘Development of new self-calibrating fluorescent sensing methods has been a popular research field with the aim of protecting the human health and environment sustainability. In this work, a novel Eu-based metal organic framework(MOF) Eu(2,6-NDC)(COO)(BUC-88) was developed by employing 2,6-NDC(2,6-naphthalenedicarboxylic acid) as bridging ligands. BUC-88 performed different sensing process toward quinolone antibiotics and tetracyclines antibiotics in terms of fluorescence intensity and color. BUC-88exhibited excellent selectivity and sensitivity detection property toward enrofloxacin(ENR), norfloxacin(NOR) and ciprofloxacin(CIP) over other Pharmaceutical and Personal Care Products(PPCPs), accomplishing the detection limit of 0.12 μmol/L, 0.52 μmol/L, 0.75 μmol/L, respectively. Notably, BUC-88 acted as an excellent fluorescence sensor for tetracyclines antibiotics with fast response time(less than 1 s), high selectivity and sensitivity(LODs = 0.08 μmol/L). The fluorescent detection method was successfully used for visual and ultrasensitive detection of ENR, NOR, CIP and tetracycline hydrochloride(TC) in lake water with satisfied recovery from 99.75% to 102.30%. Finally, the photoinduced electron transfer and the competitive absorption of ultraviolet light are the main mechanisms for sensitive detection toward quinolone antibiotics and tetracyclines antibiotics.
