The invention relates to a method for detecting the content of an
etimicin sulfate raw material and preparation of the
etimicin sulfate raw material and relevant substances. The method adopts
precolumn derivatization, the
derivatization condition comprises taking 4ml sample with appropriate concentration, adding 1ml O phthalic
aldehyde (OPA) solution into the sample, diluting the
mixed solution with
isopropyl alcohol to 10ml, heating the
mixed solution at 30-60 DEG C in water bath away from light, and obtaining
derivatization solution. The novel method for detecting
etimicin sulfate adopts a high efficiency liquid chromatograph, the chromatographic condition is that an octadecylsilane chemically bonded silica filler
chromatographic column has particle size
ranging from 4-10mum, column specification is 150-250mmX4.6-8.0mm; flowing phase is divided into organic phase and aqueous phase, wherein the
volume rate of the organic phase to the aqueous phase is 55-75:45-25, the organic phase is methyl
alcohol or
acetonitrile, the aqueous phase is glacial
acetic acid containing 0.01M-0.03M
ion pair
reagent sodium heptanesulfonate, potential of
hydrogen (PH) range is adjusted by
ammonia water or
ammonium acetate; flow speed is 0.5-1.0ml / min; sample feeding amount is 10-20mul; a
detector is a conventional
ultraviolet-visible
light detector, and detection
wavelength is from 330-350nm. The novel method for detecting etimicin
sulfate adopts the conventional
detector and the high efficiency liquid chromatograph, can achieve on-line detection of the content of the etimicin
sulfate, the preparation of the etimicin
sulfate and the relevant substances, and is simple, convenient, feasible, accurate and reliable.