ABSTRACT
Aim To determine the distribution of succinylcholine chloride (Suc) at toxic dose in rats by establishing UHPLC-MS/MS analysis. Methods The rats were subcutaneously injected with three doses of Suc, and 4 h later, rat serum and major organs were taken for acetonitrile protein precipitation and purified by solid phase extraction with WCX column. Luna NH2 column (2 mm × 100 mm, 3 μm) was used for chromatography. The mobile phase was 0. 1% formic acid-acetonitrile isoelution. Mass spectrometry was carried outwith positive ion scanning multi-reaction monitoring mode (MRM). Qualitative and quantitative analysis was conducted on the ion pairs of Suc (m/z 145. 1→93.3, m/z 145.1→115.4). Results The detection limit of Suc was 0.01 μg · L-1, the recovery rate was 89. 5% ∼ 95. 4%, and the intraday and mtraday RSD was less than 15%. Except in the untreated rat, Suc was detected in the serum, heart, liver, kidney and other major organs from Sue-administered rats, and Suc content in the kidney was the highest among organs. Conclusions Sucat poisoning dose is distributed in the serum, heart, liver, kidney and other tissues. The content in the kidney is the highest; UHPLC-MS/ MS analysis is an effective and reliable method for detecting the drug content in Sue-poisoned rats.
ABSTRACT
OBJECTIVE:To establish the method for the identification of impurities in succinylcholine chloride raw material. METHODS:Two-dimensional UPLC-QTOF-MS was adopted. One dimension chromatographic condition was Hypersil GOLD C18 column using buffer solution(22 mmol/L sodium pentanesulfonate+50 mmol/L sodium chloride+5 mmol/L sulphuric acid)as mobile phase A and acetonitrile as mobile phase B,volume ratio of mobile phase A to mobile phase B 95:5,column temperature of 40 ℃,flow rate of 1.0 mL/min,detection wavelength of 214 nm. Two-dimension chromatographic condition was ACQUITY UPLC BEH C18column using 0.1% ammonia as mobile phase A and acetonitrile as mobile phase B(gradient elution)with column temperature of 30 ℃ at flow rate of 0.4 mL/min. Ionization mode was ESI+ with capillary voltage of 2.5 kV,source temperature of 120 ℃,temperature of atomizing gas at 450 ℃,flow rate of atomizing gas at 900 L/h,acquisition mode of MSE. RESULTS:The succinic acid,succinyl chloride(intermediate),pyridine(reagent)and other impurities were detected in succinylcholine chloride by one dimensional method of HPLC. Other 4 obvious unknown impurities were named impurity 1,impurity 2,impurity 3 and impurity 4,among which the apparent content of impurity 2 was the highest. Two-dimensional method of HPLC-QTOF-MS deduced that the impurity 2 was dehydrogenate succinylcholine chloride and impurity 4 was succinylcholine chloride. The impurity 1 and impurity 3 were not detected in mass spectrum. CONCLUSIONS:Establish method for the identification of impurity in succinylcholine chloride raw material,and the results of research are used for the evaluation of the quality of the succinylcholine chloride raw material.
ABSTRACT
The use of succinylcholine chloride(Anectin(R)) prior to intubation, can cause increased contracture of ocular muscles. Therefore the authors studied the change of the squint angle under general anesthesia using pancronium bromide (Myoblock(R)) in 81 horizontal strabismus patients who had no neurologic disease and mechanical restrictions of eye movement. We used the alternative cover test and Krimsky method to measure the eye position under general anesthesia.