双胶束电动毛细管色谱测定复方化学消毒剂中聚六亚甲基单胍、聚六亚甲基双胍、醋酸洗必泰和苄索氯铵

建立了双胶束电动毛细管色谱(MEKC)分离测定复方化学消毒剂中有效成分聚六亚甲基单胍(PHMG)、聚六亚甲基双胍(PHMB)、醋酸洗必泰(CHA)及苄索氯铵(BTC)的新方法。以50.2 cm(有效长度:40 cm)×50 μm i.d.未涂层熔融石英毛细管为分离柱,20 mmol/L硼砂+30 mmol/L十二烷基硫酸钠(SDS)+5 mmol/L脱氧胆酸钠(SD)+0.8 g/L聚乙二醇 20000为分离缓冲溶液。详细研究了分离缓冲溶液中各组分浓度、样品提取液对分离的影响。4种物质的检出限和定量限均分别为1 mg/L和3 mg/L。4种物质的校正峰面积与相应质量浓度在3~140 mg/L范围内,均具有良好的线性关系,相关系数均大于0.999。回收率在84.1%~109.6%间,相对标准偏差(RSD)均低于6%。用该法测定了11件复方化学消毒剂样品中PHMG、PHMB、CHA和BTC,与产品标识值基本吻合。该法可成功区分单胍与双胍,且操作简单,适用于消毒产品的质量监督。

Determination of polyhexamethylene guanide,polyhexamethylene biguanide,chlorhexidine acetate and benzethonium chloride in compound chemical disinfectants by micellar electrokinetic chromatography with bi-micelle

A new method for the accurate assay of four components (polyhexamethylene guanide (PHMG), polyhexamethylene biguanide (PHMB), chlorhexidine acetate (CHA) and benzethonium chloride (BTC)) in compound chemical disinfectants by micellar electrokinetic chromatography (MEKC) with bi-micelle was developed. An uncoated fused-silica capillary with 50 μm i.d. and 50.2 cm total length (effective length: 40 cm) under a separation voltage of 24 kV was used. The separation buffer consisted of 20 mmol/L Na₂B₄O₇, 30 mmol/L sodium dodecyl sulfate (SDS), 5 mmol/L sodium deoxycholate (SD) and 0.8 g/L polyethyleneglycol (PEG) 20000. A 1 : 10 dilution of the running buffer with ultrapure water was used as the sample buffer. The injection pressure and time were 3.448 kPa and 12 s, respectively. Liquid samples could be directly injected after dilution with sample buffer. Solid samples were extracted with 10 mL of sample buffer twice and the two extracted solutions were merged together and then directly injected. The factors such as the buffer concentration and pH, the concentrations of SDS and SD, the concentration of PEG 20000 and the sample extraction solution which influence the separation were investigated in detail. The corrected peak areas versus the concentrations of the four components showed good linear relationships within the range from 3 mg/L to 140 mg/L with correlation coefficients (r) greater than 0.999. The limits of detection (LODs) and the limits of quantification (LOQs) of the four components were all 1 mg/L and 3 mg/L, respectively. The average recoveries at three spiked levels were in the range of 84.1%-109.6% with RSDs all less than 6%. Eleven samples were analyzed and the results met well with the specified content. The PHMG could be easily discriminated from PHMB. The MEKC method is suitable for the supervision of compound chemical disinfectants.