CN201711085814.X reported a detection method for octyl p-methoxycinnamate in textiles, comprising the following steps:
The first step, sampling from the textile: use stainless steel scissors to cut the sample into small rectangular pieces with a diagonal length not greater than 5mm.
In the second step, 1.0 g of the chopped sample was weighed and placed in a 40 mL container (reaction tube in this example), then 10 mL of methanol was added to the container, and the container was placed in an ultrasonic cleaner for ultrasonic extraction for 30 min. Ultrasonic frequency is 50kHz, ultrasonic temperature is 25 ℃, obtains extract;
In the third step, the extract obtained in the second step is filtered to obtain the liquid to be tested. Specifically, 1 mL of the extract is filtered with a 0.45 μm organic filter membrane into a sample bottle;
In the fourth step, the liquid to be tested obtained in the third step is analyzed by an ultra-high performance liquid chromatography tandem mass spectrometer (UPLC-MSMS). Wherein, the model of the ultra-high performance liquid chromatography tandem mass spectrometer is WatersAcquityHClass+XevoTQD, and the chromatographic column model is WatersBEHC18 column, and the specification of the chromatographic column is 50mm×2.1mm×1.7μm (column length is 50mm, and the particle size of the filler is 50mm×2.1mm×1.7μm). is 1.7 μm, and the inner diameter of the column is 2.1 mm).
The test conditions of the ultra-high performance liquid chromatography tandem mass spectrometer are: the injection volume is 5 μl; the flow rate is 0.2 mL/min; the elution process adopts the gradient elution procedure; the acquisition mode is the positive ion MRM mode; the capillary voltage is 0.5KV; the desolvation gas flow rate is 900L/h; the desolvation gas temperature is 400°C; the parent ion is 291.1, the cone voltage is 15V, the quantitative product ion is 179.1, and the collision energy is 8V; the qualitative product ion is 161.1, and the collision energy is 15V; quantitative transition 291.1→179.1, qualitative transition 291.1→161.1.
Specifically, the gradient elution procedure is shown in Table 1:
Table 1: Gradient elution procedure.
The flow rate of gradient elution was 0.2 mL/min.
By adopting the method of the invention, octyl p-methoxycinnamate and impurities can be efficiently separated, and the qualitative and quantitative analysis of octyl p-methoxycinnamate can be carried out quickly and accurately.
