Ultrasonic-assisted supercritical fluid separation removing plasticizers from ganoderma lucidum spores’ oil (2024)

Keywords: Ganoderma lucidum spores’ oil, Plasticizer, Triterpenes, Ultrasonic-assisted supercritical fluid separation, Nanofiltration

2.1. Materials

Oleanolic acid reference substance (purity ≥91.1%), DBP reference substance (purity ≥99.8%) and DEP reference substance (purity ≥99.5%) were purchased from the National Institute for Food and Drug Control (Beijing, China). Ganoderic acid A reference substance (purity ≥98.0%) was obtain from nanjing Dilger Medical Technology Co., Ltd. (Nanjing, China). Ganoderma lucidum spore powder was provided by Jiangsu Hongshou Biological Engineering Co., Ltd. (Nantong, China). CO₂ (purity ≥99.9%) was obtain from Nanjing Guanghua Gas Company (Nanjing, China). Acetonitrile was chromatographic grade and and got from Merck (Darmstadt, Germany). Glacial acetic acid, vanilla aldehyde, perchloric acid, anhydrous ethanol and other chemicals were all analytical grade and purchased from Sinopharm group chemical reagent Co. Ltd. (Shanghai, China).

2.2. USFS system

The SFE apparatus and the ultrasonic generator made up the USFS system, as shown in Fig. 1. A control panel, CO₂ steel vessel, CO₂ deposit tank, pressure pump, flow meter, cold trap, extraction vessel, primary separation kettle, and secondary separation kettle were all included in the SFE equipment (mode: HA-120-50-01-C) which was purchased from Nantong Huaan Supercritical Fluid Extraction Co. Ltd. In addition, there was a maximum operating pressure of 60MPa and a temperature limit of 150°C. Oil baths were used to heat the extraction vessel, and flowing water was used to regulate the temperature of the separating vessel. Through the control panel, the SFE settings could be changed, and the flow rate, temperature, and pressure could all be kept within 0.1L/min, 0.1°C, and 0.1MPa, respectively. The QD-T6A ultrasonic generator, which was purchased from Jidao company and installed at the entrance of the primary separation kettle, provides adjustable continuous power outputs at a fixed frequency of 40kHz. The ultrasonic power can be changed between 0–1, 200W at the same time.

2.3. USFS plasticizers from ganoderma lucidum spore powder

The extraction parameters, which were determined from industrial production of businesses, were as follows: temperature of 45.0°C, pressure of 38.0MPa, and CO₂ flow rate of 40.0 L/h. Ganoderma lucidum spore powder was placed in the extraction vessel. In the meantime, the secondary separation kettle's separation parameters are as follows: temperature of 25.0°C, pressure of 5.0MPa. Experiments were conducted at various separation temperatures (5.0–40.0°C), pressures (5.0–30.0MPa), and ultrasonic powers (0–800W) in order to better understand the effectiveness of the separation between triterpenoids and plasticizers in the main separation kettle. The primary separation kettle's operational conditions for the single factor experiment were set as follows: temperature of 20.0°C, pressure of 10.0MPa, and ultrasonic power of 200W.

In order to evaluate the viability of process parameters, triterpenoids and plasticizer content in the primary separation kettle were detected and calculated after USFS plasticizers from ganoderma lucidum spore powder.

2.4. Conventional SFE

According to USFS, the operating parameters of extraction vessel and secondary separation kettle were consistent with USFS. The separation parameters of primary separation kettle refer to the optimal parameters of USFS without ultrasound.

2.5. Sample analysis

2.6. Experiment design and statistical analysis

Response surface methodology (RSM) was a mathematical technique for quickly and efficiently planning and optimizing the technological parameters in the medicine and food industries. Temperature (X₁), pressure (X₂), and ultrasonic power (X₃) were chosen as the factors to build the response surface experiment based on the findings of the single factor experiment [21], [22], [23]. In order to find the ideal separation conditions for USFS, a three-variable, three-level experiment with 17 experimental runs was conducted. Each run of experiments was performed three times in order to get the average value.

The contents of triterpenoids and plasticizers were selected as response value (Y) to calculate the correlation equation with the investigated variables (Xi) by quadratic polynomial model. As shown in Equation (2), the quadratic polynomial equation was used to predict the response by taking the variables into account. The statistical significance of the equation was examined by the analysis of variance (ANOVA), and the significance of each variable and interaction between variables were calculated by the P-value.

where a₀ is the constant; a_i is the linear regression coefficient; a_ii is the quadratic regression coefficient; a_ij is the interaction regression coefficient; X_i and X_j are independent variables.

2.7. Analysis of the plasticizers' release from spores oil

In order to evaluate the theory that ultrasonic treatment causes the release of plasticizers from spores oil and confirm the USFS separation mechanism. Using the molecular weight difference between triterpenoids and plasticizers as a guide, nanofiltration technology was chosen to separate the ethanol solution of ganoderma lucidum spores’ oil that had been extracted using conventional SFE [24]. Ganoderma lucidum spores’ oil was stirred and diluted to a concentration of 0.050g/mL using a methanol solution, and then filtrated by nanofiltration apparatus with a molecular weight cutoff 800Da membrane (Synder Corporation, USA). The SCQ-9200E ultrasonic apparatus (Shengyan Corporation, China) was used in the nanofiltration separation process with ultrasonic powers ranging from 0W to 500W for the ganoderma lucidum spores’ oil methanol solution. The transmittance (T) being computed using Equation (3).

where C₁ and C₂ are the solute concentrations in filtration solution and original solution.

3.1. Single factor test

3.2. Statistical analysis and model fitting using RSM

17 experiments (12 factorial and 5 central) were designed and carried out by Box-Behnken design of RSM, which was applied to optimize USFS conditions and explore the separation mechanism between plasticizer and triterpenes. The separation results of total triterpenes, ganoderic acid A, DBP and DEP were shown in Table 1, the content of total triterpenes and ganoderic acid A ranged from 6.06g to 6.95g and 0.71g to 1.15g, respectively. Compared to the highest content under USFU, the loss of total triterpenes and ganoderic acid A was 12.81% and 38.26% accordingly. Meanwhile, the contents of DBP and DEP ranged from 0.022mg to 0.810mg and 0.010mg to 0.429mg, respectively, some of which exceed the content limit of 0.3mg. As a result, based on the rule of the influence of variables on the content of index components, it is required to optimize the separation parameters suited for production.

As a result, the relationship between content and variables was described by the quadratic polynomial equation.

$$\mathrm{T}\mathrm{o}\mathrm{t}\mathrm{a}\mathrm{l}\mathrm{t}\mathrm{r}\mathrm{i}\mathrm{t}\mathrm{e}\mathrm{r}\mathrm{p}\mathrm{e}\mathrm{n}\mathrm{e}\mathrm{s}\mathrm{c}\mathrm{o}\mathrm{n}\mathrm{t}\mathrm{e}\mathrm{n}\mathrm{t}\left(Y_1,\mathrm{g}\right)=6.71-0.23X_1-0.12X_2-0.14X_3+0.037X_1{X}_2-0.095X_1{X}_3$$

$$+0.022X_2{X}_3-0.048X_1^2-0.090X_2^2-0.12X_3^2(4)$$

$$\mathrm{G}\mathrm{a}\mathrm{n}\mathrm{o}\mathrm{d}\mathrm{e}\mathrm{r}\mathrm{i}\mathrm{c}\mathrm{a}\mathrm{c}\mathrm{i}\mathrm{d}\mathrm{A}\mathrm{c}\mathrm{o}\mathrm{n}\mathrm{t}\mathrm{e}\mathrm{n}\mathrm{t}\left(Y_2,\mathrm{g}\right)=0.99-0.12X_1-0.043X_2-0.069X_3+0.02X_1{X}_2-0.033X_1{X}_3$$

$$-0.02X_2{X}_3-0.024X_1^2-0.006X_2^2-0.039X_3^2(5)$$

$$\mathrm{D}\mathrm{B}\mathrm{P}\mathrm{c}\mathrm{o}\mathrm{n}\mathrm{t}\mathrm{e}\mathrm{n}\mathrm{t}\left(Y_3,\mathrm{m}\mathrm{g}\right)=0.041-0.037X_1-0.15X_2-0.18X_3+0.011X_1{X}_2+0.017X_1{X}_3$$

$$+0.11X_2{X}_3+0.055X_1^2+0.11X_2^2+0.20X_3^2(6)$$

$$\mathrm{D}\mathrm{E}\mathrm{P}\mathrm{c}\mathrm{o}\mathrm{n}\mathrm{t}\mathrm{e}\mathrm{n}\mathrm{t}\left(Y_4,\mathrm{m}\mathrm{g}\right)=0.026-0.030X_1-0.075X_2-0.090X_3+0.001X_1{X}_2+0.035X_1{X}_3$$

$$+0.070X_2{X}_3+0.014X_1^2+0.060X_2^2+0.094X_3^2(7)$$

The F-value, P-value, lack of fit and R-square were selected to evaluate the feasibility of the model and the interaction between factors by ANOVA. The model term was significant when the P-value was less than 0.05. And the P-value of lack of fit was >0.05 implied the lack of fit was not significant relative to the pure error. The results of ANOVA for response surface quadratic model were shown in Table 2, the P-value of model was less than 0.05, indicating the regressions for the contents of four indexes were statistically significant. The four significant terms common to all indexes were X₁, X₂, X₃ and X₃². On the other hand, X₁X₃ was a significant common term in the two regressions that used total triterpenes, ganoderic acid A and DEP content, X₂X₃ was a significant common term in the two regressions that used DBP and DEP content, X₁² was a significant common term in two regressions that used ganoderic acid A and DBP content, and X₂² was a significant common term in those regressions that used total triterpenes, DBP and DEP content. Finally, X₁X₂ was the only insignificant common term in all regressions. The results showed that DBP and DEP were X₃>X₂>X₁, whereas total triterpenes and ganoderic acid A were X₁>X₃>X₂. This provided a strategy for removing plasticizers from ganoderma lucidum triterpenes. Additionally, the lack of fit's P-value was higher than 0.05, indicating that it was unimportant compared to the pure error.

Table 3 shows the statistical tests for the four models, the predicted R² was in reasonable agreement with the adjusted R², which indicated the experimental values could be significantly predicted by the model. The C.V. values were 0.68––16.74%, indicated that the variance of the response variable was relatively small and the experimental results were stable. And all of the models’ standard deviations were lower than their means, which explains the decreased variability between the models and experimental results. In addition, the adequate precision of four indexes were bigger than 4, indicated all the models could be used to navigate the design space.

In order to illustrate the interactive effects between each variable (temperature, pressure and ultrasonic power) on removing plasticizer from triterpenes while setting the third variable constant, the three-dimensional response surface plots were used as Fig. 3, Fig. 4, Fig. 5, Fig. 6. Fig. 3b exhibits the interactive effects between X₁ (temperature) and X₃ (ultrasonic power) on the content of total triterpenes, while keeping the pressure constant at 17.5MPa. The content of total triterpenes decreased with the increasing of temperature and pressure, which was consistent with the supercritical extraction theory. The solubility of total triterpenes in supercritical CO₂ fluids increases with the increase of temperature, resulting in a decrease of precipitation in the separation kettle. And the solubility of total triterpenes in supercritical fluids can be adjusted by ultrasound. The interactions between X₁ (temperature) and X₂ (pressure) was investigated when ultrasonic power was constant, the content of total triterpenes was nearly unchanged. The similar result was found in the interactions between X₂ (pressure) and X₃ (ultrasonic power), therefore, the interactions of X₁X₂ and X₂X₃ was insignificant. As a representative component of total triterpenes of ganoderma lucidum, the interactive effects between each variable of ganoderic acid A were similar to total triterpenes (Fig. 4).

The interactive effects between each variable of DBP were shown in Fig. 5, the interactions between X₂ (pressure) and X₃ (ultrasonic power) was investigated when temperature was constant at 25 ℃. It can be observed that a decrease in pressure and ultrasonic power increases the DBP content. But the lowest value of content was close to 0 with the increasing of ultrasonic power from 280W to 440W and pressure from 17.5MPa to 25MPa. The experimental finding shows that when ultrasonic was used to reduce the size of spores oil droplets, DBP molecules were liberated from the spores oil and redissolved in supercritical CO₂ fluid [29], [30]. However, once the ultrasonic power above 440W, the solubility of DBP in supercritical CO₂ fluid decreased and DBP molecules precipitated in the primary separation kettle. The interaction between X₁ (temperature) and X₂ (pressure), X₁ (temperature) and X₃ (ultrasonic power) were not significant. The results supported the conclusions drawn from the ANOVA results.

The impact of operational variables on DEP content in the RSM method is shown in Fig. 6. The interaction of X₁X₃ has a significant influence on DEP content because DEP has a smaller molecular weight than DBP and the effect of temperature on the release of DEP is more pronounced under the ultrasonic-assisted effect. Compared to DBP and ganoderma lucidum triterpenoids, DEP is more vulnerable to the interaction effect of ultrasonic power and supercritical pressure. When DEP is separated from spores oil using ultrasonic, the amount of DEP in the primary separation kettle decreases and it may be dissolved in supercritical fluid more easily. The interaction between X₁ (temperature) and X₂ (pressure) was not significant. The results of the experiment confirmed the inferences made based on the ANOVA findings.

According to the model, the optimal conditions were as follows: temperature of 15.24°C, pressure of 17.96MPa, and ultrasonic power of 363.91W. This was accomplished by balancing the separation of plasticizers and the triterpenoids from ganoderma lucidum. The target values of total triterpenes, ganoderic acid A, DBP, and DEP were predicted by the model to be 6.85g, 1.06g, 0.08mg, and 0.03mg, respectively, under optimal conditions.

Verification experiments were carried out under the optimal conditions of temperature of 15.0°C, pressure of 18.0MPa, and ultrasonic power of 360W to confirm the accuracy of the response model. Total triterpenes, ganoderic acid A, DBP, and DEP all had experimental contents of 6.89g, 1.10g, 0.09mg, and 0.04mg. Meanwhile, DBP and DEP concentrations were below the required content level. Plasticizers were challenging to get out of ganoderma lucidum spores’ oil, as was previously mentioned. When looking for the best USFS technique to remove DBP and DEP from ganoderma lucidum spores’ oil, RSM was accurate and dependable as seen by the similarity between experimental results and projected values.

3.3. Comparison of USFS with conventional SFE

The primary separation kettle's contents of total triterpene content, ganoderic acid A, DBP, and DEP were utilized as indexes to evaluate the separation effectiveness of USFS compared to conventional SFE in accordance with RSM's recommended parameters. Under conventional SFE, the experimental contents of total triterpenes and ganoderic acid A were 6.86g and 1.12g, respectively, which are equivalent to the USFS. Due to their larger molecular weight and oil–water partition coefficient (LogP), DBP and DEP are more soluble in supercritical CO₂ fluids than triterpenoids. Table 4 demonstrates that the experimental DBP and DEP levels were significantly higher than USFS at 1.31mg and 0.63mg, respectively. Additionally, the contents of DBP and DEP were reduced by changing the supercritical pressure and temperature in the primary separation kettle, and the triterpenoids were also reduced. The content of total triterpenes and ganoderic acid A was 0.12g and 0.03g, respectively, as the content of DBP and DEP was less than 0.10mg utilizing the supercritical temperature of 40.0°C and pressure of 35.5MPa. Meanwhile, the ganoderma lucidum spores’ oil was released from supercritical CO₂ fluid in the secondary separation kettle, and the contents of DBP and DEP were significantly higher than USFS. As a result, it proved difficult to resolve the conflict of triterpenoids and plasticizers separated by conventional SFE.

3.4. Nanofiltration separation with ultrasound

In Table 5, which summarizes the results of the nanofiltration separation of ganoderma lucidum spores’ oil, it is evident that the transmittances of DBP and DEP were comparable to those of total triterpenes and ganoderic acid A without ultrasound, contradicting the sieving theory of nanofiltration [31]. DBP and DEP had significantly higher transmittances than total triterpenes and ganoderic acid A when ultrasonic powers increased. The transmittances of the four indexes also increased significantly. The increasing trend of DBP and DEP transmittances tended to remain steady when the ultrasonic power approaches 300W, whereas total triterpenes and ganoderic acid A transmittances grew gradually. The findings demonstrated that triterpenoids and plasticizers existed in ganoderma lucidum spores’ oil despite being dissolved in a methanol solution. Small molecules of plasticizers were gradually dissolved in a methanol solution under the combined effects of ultrasonic cavitation and acoustic streaming, and then passed through a nanofiltration membrane in accordance with the pore size sieving effect [32], [33]. The van der Waals forces of triterpenoids were greater than those of plasticizers. As a result, the transmittances of triterpenoids increased steadily.

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